Synthesis evidence

Cu/Co bimetallic conductive MOFs: Electronic modulation for enhanced nitrate reduction to ammonia

Liu P., Yan J., Huang H. et al. · Chemical Engineering Journal · 2023 · 143134

5 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Hydrothermal

2 · 2.2 Synthetic procedures · Table 1

Metal precursorsCu(OAc)2.H2O and/or Co(OAc)2.4H2O according to Table 1
Linker precursorsHHTP
Solvents5 mL ultrapure water for metal salt; 5 mL DMF for HHTP/NH4OH
Additives0.12 mL aqueous ammonia (NH4OH, 28% NH3)
Atmospherenot specified
Temperature85
Time2
Substrate orientationnot applicable
Oxidant / reductantnone specified
Work-upnatural cooling; washed with deionized water and acetone 6 times respectively; vacuum dried at 60 C overnight
Activationvacuum oven drying at 60 C overnight
Scalability context20 mL beaker batch; no scale-up data reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCupric acetate monohydrate (Cu(OAc)2.H2O)0 mg2 · 2.2 Synthetic procedures · Table 1
Metal SourceCobalt acetate tetrahydrate (Co(OAc)2.4H2O)100.0 mg2 · 2.2 Synthetic procedures · Table 1
Linker2,3,6,7,10,11-hexahydroxytriphenylene hydrate (HHTP)65 mg2 · 2.2 Synthetic procedures · Table 1
Solventultrapure water5 mL2 · 2.2 Synthetic procedures · Table 1
SolventN,N-dimethylformamide (DMF)5 mL2 · 2.2 Synthetic procedures · Table 1
Baseaqueous ammonia0.12 mL · 28% NH32 · 2.2 Synthetic procedures · Table 1
Complete recipeSource: Main

Route 2: Hydrothermal

2 · 2.2 Synthetic procedures · Table 1

Metal precursorsCu(OAc)2.H2O and/or Co(OAc)2.4H2O according to Table 1
Linker precursorsHHTP
Solvents5 mL ultrapure water for metal salt; 5 mL DMF for HHTP/NH4OH
Additives0.12 mL aqueous ammonia (NH4OH, 28% NH3)
Atmospherenot specified
Temperature85
Time2
Substrate orientationnot applicable
Oxidant / reductantnone specified
Work-upnatural cooling; washed with deionized water and acetone 6 times respectively; vacuum dried at 60 C overnight
Activationvacuum oven drying at 60 C overnight
Scalability context20 mL beaker batch; no scale-up data reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCupric acetate monohydrate (Cu(OAc)2.H2O)40 mg2 · 2.2 Synthetic procedures · Table 1
Metal SourceCobalt acetate tetrahydrate (Co(OAc)2.4H2O)50 mg2 · 2.2 Synthetic procedures · Table 1
Linker2,3,6,7,10,11-hexahydroxytriphenylene hydrate (HHTP)65 mg2 · 2.2 Synthetic procedures · Table 1
Solventultrapure water5 mL2 · 2.2 Synthetic procedures · Table 1
SolventN,N-dimethylformamide (DMF)5 mL2 · 2.2 Synthetic procedures · Table 1
Baseaqueous ammonia0.12 mL · 28% NH32 · 2.2 Synthetic procedures · Table 1
Complete recipeSource: Main

Route 3: Hydrothermal

2 · 2.2 Synthetic procedures · Table 1

Metal precursorsCu(OAc)2.H2O and/or Co(OAc)2.4H2O according to Table 1
Linker precursorsHHTP
Solvents5 mL ultrapure water for metal salt; 5 mL DMF for HHTP/NH4OH
Additives0.12 mL aqueous ammonia (NH4OH, 28% NH3)
Atmospherenot specified
Temperature85
Time2
Substrate orientationnot applicable
Oxidant / reductantnone specified
Work-upnatural cooling; washed with deionized water and acetone 6 times respectively; vacuum dried at 60 C overnight
Activationvacuum oven drying at 60 C overnight
Scalability context20 mL beaker batch; no scale-up data reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCupric acetate monohydrate (Cu(OAc)2.H2O)26.6 mg2 · 2.2 Synthetic procedures · Table 1
Metal SourceCobalt acetate tetrahydrate (Co(OAc)2.4H2O)66.7 mg2 · 2.2 Synthetic procedures · Table 1
Linker2,3,6,7,10,11-hexahydroxytriphenylene hydrate (HHTP)65 mg2 · 2.2 Synthetic procedures · Table 1
Solventultrapure water5 mL2 · 2.2 Synthetic procedures · Table 1
SolventN,N-dimethylformamide (DMF)5 mL2 · 2.2 Synthetic procedures · Table 1
Baseaqueous ammonia0.12 mL · 28% NH32 · 2.2 Synthetic procedures · Table 1
Complete recipeSource: Main

Route 4: Hydrothermal

2 · 2.2 Synthetic procedures · Table 1

Metal precursorsCu(OAc)2.H2O and/or Co(OAc)2.4H2O according to Table 1
Linker precursorsHHTP
Solvents5 mL ultrapure water for metal salt; 5 mL DMF for HHTP/NH4OH
Additives0.12 mL aqueous ammonia (NH4OH, 28% NH3)
Atmospherenot specified
Temperature85
Time2
Substrate orientationnot applicable
Oxidant / reductantnone specified
Work-upnatural cooling; washed with deionized water and acetone 6 times respectively; vacuum dried at 60 C overnight
Activationvacuum oven drying at 60 C overnight
Scalability context20 mL beaker batch; no scale-up data reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCupric acetate monohydrate (Cu(OAc)2.H2O)53.4 mg2 · 2.2 Synthetic procedures · Table 1
Metal SourceCobalt acetate tetrahydrate (Co(OAc)2.4H2O)33.3 mg2 · 2.2 Synthetic procedures · Table 1
Linker2,3,6,7,10,11-hexahydroxytriphenylene hydrate (HHTP)65 mg2 · 2.2 Synthetic procedures · Table 1
Solventultrapure water5 mL2 · 2.2 Synthetic procedures · Table 1
SolventN,N-dimethylformamide (DMF)5 mL2 · 2.2 Synthetic procedures · Table 1
Baseaqueous ammonia0.12 mL · 28% NH32 · 2.2 Synthetic procedures · Table 1
Complete recipeSource: Main

Route 5: Hydrothermal

2 · 2.2 Synthetic procedures · Table 1

Metal precursorsCu(OAc)2.H2O and/or Co(OAc)2.4H2O according to Table 1
Linker precursorsHHTP
Solvents5 mL ultrapure water for metal salt; 5 mL DMF for HHTP/NH4OH
Additives0.12 mL aqueous ammonia (NH4OH, 28% NH3)
Atmospherenot specified
Temperature85
Time2
Substrate orientationnot applicable
Oxidant / reductantnone specified
Work-upnatural cooling; washed with deionized water and acetone 6 times respectively; vacuum dried at 60 C overnight
Activationvacuum oven drying at 60 C overnight
Scalability context20 mL beaker batch; no scale-up data reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCupric acetate monohydrate (Cu(OAc)2.H2O)80 mg, 0.4 mmol2 · 2.2 Synthetic procedures · Table 1
Metal SourceCobalt acetate tetrahydrate (Co(OAc)2.4H2O)0 mg2 · 2.2 Synthetic procedures · Table 1
Linker2,3,6,7,10,11-hexahydroxytriphenylene hydrate (HHTP)65 mg, 0.2 mmol2 · 2.2 Synthetic procedures · Table 1
Solventultrapure water5 mL2 · 2.2 Synthetic procedures · Table 1
SolventN,N-dimethylformamide (DMF)5 mL2 · 2.2 Synthetic procedures · Table 1
Baseaqueous ammonia0.12 mL · 28% NH32 · 2.2 Synthetic procedures · Table 1