Synthesis evidence

Novel semiconducting iron–quinizarin metal–organic framework for application in supercapacitors*

Agrawal S., Clarke S.M., Vitorica-Yrezabal I.J. et al. · Molecular Physics · 2019 · 3424-3433

2 structured synthesis routes

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

Vague recipeSource: Main

Route 1: Other

p008 · 4. Results

Metal precursorsas-synthesised FeQ
Linker precursorsas-synthesised FeQ
Solventssolvent exchange solvent not reported
Atmospherein vacuo during heating
Temperaturenot reported
Timenot reported
Work-upsolvent exchange followed by heating in vacuo
Activationsolvent exchange followed by heating in vacuo
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Otheras-synthesised FeQnot reportedp008 · 4. Results
Partial recipeSource: Main

Route 2: Solvothermal

p007 · 3. FeQ synthesis

Metal precursorsIron(II) acetate (86.97 mg, 0.5 mmol)
Linker precursorsquinizarin / 1,4-dihydroxyanthraquinone (120.1 mg, 0.5 mmol)
Solventswater (5 mL) plus ethanol (5 mL), 1:1 water-ethanol mixture
Atmospherenot reported for synthesis
Temperature175; then 90
Time72 h at 175 deg C; cooled to 90 deg C at 6 deg C/h; 48 h at 90 deg C; then cooled to room temperature
Substrate orientationnone; bulk autoclave synthesis
Oxidant / reductantnot reported
Work-upfiltered under vacuum; washed with hot ethanol and acetone; black precipitate obtained
ActivationFor the activated BET sample the paper states solvent exchange followed by heating in vacuo, but gives no activation solvent, temperature or time.
Scalability contextProduct obtained only in 1:1 water-ethanol; pure water or pure ethanol did not give FeQ. Authors note deposited layers on substrates remain a challenge.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceIron(II) acetate86.97 mg, 0.5 mmolp007 · 3. FeQ synthesis
Linkerquinizarin120.1 mg, 0.5 mmolp007 · 3. FeQ synthesis
Solventwater5 mLp007 · 3. FeQ synthesis
Solventethanol5 mLp007 · 3. FeQ synthesis