cMOF Evidence Base

Synthesis evidence

Ultrathin two-dimensional π-d conjugated coordination polymer Co3(hexaaminobenzene)2 nanosheets for highly efficient oxygen evolution

Li C., Shi L., Zhang L. et al. · Journal of Materials Chemistry A · 2020 · 369-379

8 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

p009 / article p377 · Synthesis of catalysts

Metal precursorscobalt nitrate hexahydrate [Co(NO3)2.6H2O]
Linker precursorsHAB
Solventswater; deoxygenated water
Additivesaqueous ammonium hydroxide (NH4OH)
AtmosphereHAB solution in deoxygenated water; otherwise not stated
Temperatureroom temperature reaction; vacuum drying at 80 C
Time2 h reaction; overnight drying
Work-upfiltered, washed with water and acetone
Activationdried under vacuum at 80 C overnight
Scalability contextSoft-chemistry solution route; no explicit scale-up data.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecobalt nitrate hexahydrate [Co(NO3)2.6H2O]80 mg (0.276 mmol)p009 / article p377 · Synthesis of catalysts
Solventwater10 mLp009 / article p377 · Synthesis of catalysts
Base25-28% aqueous ammonium hydroxide (NH4OH)0.78 mL (10.9 mmol) · 25-28%p009 / article p377 · Synthesis of catalysts
LinkerHAB30 mg (0.109 mmol)p009 / article p377 · Synthesis of catalysts
Solventdeoxygenated water5 mLp009 / article p377 · Synthesis of catalysts
Complete recipeSource: Main

Route 2: Other

p009 / article p377 · Synthesis of catalysts

Metal precursorsbulk Co-HAB
Linker precursorsbulk Co-HAB
AtmosphereAr
Temperature500 C
Time2 h
Oxidant / reductantthermal carbonisation under inert atmosphere
Activationheated under Ar
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Otherbulk Co-HABNot specifiedp009 / article p377 · Synthesis of catalysts
Complete recipeSource: Main

Route 3: Solvothermal

p009 / article p377 · Synthesis of catalysts

Metal precursorscobalt nitrate hexahydrate [Co(NO3)2.6H2O]
Linker precursorsHAB
SolventsDMF; water; deoxygenated water inferred from Co-HAB-NSs route
Additivesaqueous ammonium hydroxide (NH4OH)
AtmosphereTeflon autoclave; gas atmosphere not stated
Temperature40 C
Time8 h
Work-upsimilar to Co-HAB-NSs route
Activationsimilar drying to Co-HAB-NSs route implied
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecobalt nitrate hexahydrate [Co(NO3)2.6H2O]as in Co-HAB-NSs routep009 / article p377 · Synthesis of catalysts
LinkerHABas in Co-HAB-NSs routep009 / article p377 · Synthesis of catalysts
Complete recipeSource: Main

Route 4: Solvothermal

p009 / article p377 · Synthesis of catalysts

Metal precursorscobalt nitrate hexahydrate [Co(NO3)2.6H2O]
Linker precursorsHAB
SolventsDMF; water; deoxygenated water inferred from Co-HAB-NSs route
Additivesaqueous ammonium hydroxide (NH4OH)
AtmosphereTeflon autoclave; gas atmosphere not stated
Temperature100 C
Time12 h
Work-upsimilar to Co-HAB-NSs route
Activationsimilar drying to Co-HAB-NSs route implied
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecobalt nitrate hexahydrate [Co(NO3)2.6H2O]as in Co-HAB-NSs routep009 / article p377 · Synthesis of catalysts
LinkerHABas in Co-HAB-NSs routep009 / article p377 · Synthesis of catalysts
Complete recipeSource: Main

Route 5: Other

p009 / article p377 · Synthesis of catalysts

Metal precursorscobalt nitrate hexahydrate [Co(NO3)2.6H2O]
Linker precursorsHAB
SolventsDMF; water; deoxygenated water inferred from base route
Additivesaqueous ammonium hydroxide (NH4OH)
Atmospherenot stated; base route uses deoxygenated water for HAB
Temperature75 C reaction; vacuum drying at 80 C
Timesimilar to bulk route, 2 h reaction implied; overnight drying
Work-upsimilar to bulk route: filtered, washed with water and acetone
Activationsimilar to bulk route: dried under vacuum at 80 C overnight
Scalability contextAuthors call the route simple, cost-efficient, and soft-chemistry; no yield or scale-up demonstration is given for Co-HAB-NSs.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecobalt nitrate hexahydrate [Co(NO3)2.6H2O]80 mg (0.276 mmol)p009 / article p377 · Synthesis of catalysts
SolventDMF10 mLp009 / article p377 · Synthesis of catalysts
Solventwater5 mLp009 / article p377 · Synthesis of catalysts
Base25-28% aqueous ammonium hydroxide (NH4OH)0.78 mL (10.9 mmol), inherited from bulk route · 25-28%p009 / article p377 · Synthesis of catalysts
LinkerHAB30 mg (0.109 mmol), inherited from bulk routep009 / article p377 · Synthesis of catalysts
Complete recipeSource: Main

Route 6: Other

p009 / article p377 · Synthesis of catalysts

Metal precursorscobalt nitrate hexahydrate [Co(NO3)2.6H2O]
Linker precursorsHAB
Solventswater; deoxygenated water
Additivesaqueous ammonium hydroxide (NH4OH), doubled relative to bulk route
AtmosphereHAB solution in deoxygenated water; otherwise not stated
Temperatureroom temperature reaction implied from bulk route; vacuum drying at 80 C
Time2 h reaction implied; overnight drying
Work-upfiltered, washed with water and acetone
Activationdried under vacuum at 80 C overnight
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecobalt nitrate hexahydrate [Co(NO3)2.6H2O]80 mg (0.276 mmol), inherited from bulk routep009 / article p377 · Synthesis of catalysts
Base25-28% aqueous ammonium hydroxide (NH4OH)1.56 mL / 21.8 mmol inferred as doubled from 0.78 mL / 10.9 mmol · 25-28%p009 / article p377 · Synthesis of catalysts
LinkerHAB30 mg (0.109 mmol), inherited from bulk routep009 / article p377 · Synthesis of catalysts
Complete recipeSource: Main

Route 7: Solvothermal

p009 / article p377 · Synthesis of catalysts

Metal precursorscobalt nitrate hexahydrate [Co(NO3)2.6H2O]
Linker precursorsHAB
SolventsDMF; water; deoxygenated water inferred from Co-HAB-NSs route
Additivesaqueous ammonium hydroxide (NH4OH)
AtmosphereTeflon autoclave; gas atmosphere not stated
Temperature70 C
Time4 h
Work-upsimilar to Co-HAB-NSs route
Activationsimilar drying to Co-HAB-NSs route implied
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecobalt nitrate hexahydrate [Co(NO3)2.6H2O]as in Co-HAB-NSs routep009 / article p377 · Synthesis of catalysts
LinkerHABas in Co-HAB-NSs routep009 / article p377 · Synthesis of catalysts
Complete recipeSource: Main

Route 8: Other

p009 / article p377 · Synthesis of catalysts

Linker precursors4-nitroaniline; 4-amino-1,2,4-triazole; TATB intermediate
SolventsH2SO4; DMSO; aqueous HCl; aqueous HNO3; water; concentrated HCl
AdditivesKNO3; sodium methylate; NaOH; SnCl2
Temperature50 C addition; 80 C for 3 h; 110 C for 3 h; 70 C gentle heating; room temperature 2-7 days
Time3 h at 80 C; 3 h at 110 C; 3 h stirring with NaOMe; 2-7 days reduction
Oxidant / reductantKNO3 nitration; SnCl2 reduction
Work-upcooled, poured into ice water, precipitates collected/dried/recrystallised; washed with water; filtered; washed with concentrated HCl; dried; HCl added to aqueous solution to yield protonated HAB
Show 8 structured reagent records
RoleReagentAmount / concentrationSource
Linker4-nitroaniline20 gp009 / article p377 · Synthesis of catalysts
AcidH2SO4100 mL + 100 mLp009 / article p377 · Synthesis of catalysts
OxidantKNO370 gp009 / article p377 · Synthesis of catalysts
LinkerTNA4.56 gp009 / article p377 · Synthesis of catalysts
Other4-amino-1,2,4-triazole (ATA)16.8 gp009 / article p377 · Synthesis of catalysts
SolventDMSO300 mLp009 / article p377 · Synthesis of catalysts
BaseNaOMe23.8 gp009 / article p377 · Synthesis of catalysts
ReductantSnCl236.7 g (193.5 mmol, 25 eq.)p009 / article p377 · Synthesis of catalysts