Synthesis evidence

Host-guest molecular interaction promoted urea electrosynthesis over a precisely designed conductive metal-organic framework

Yuan M., Chen J., Zhang H. et al. · Energy and Environmental Science · 2022 · 2084-2095

4 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Drop Cast

p003 · Electrochemical measurements

Solvents500 uL ethanol and 470 uL water
Additives30 uL Nafion (0.5 wt%)
AtmosphereElectrodes used immediately or kept under vacuum before electrochemistry
Temperature25
Substrate orientationCarbon cloth piece, 1 x 3 cm2
Work-upCarbon cloth pretreated with H2SO4:H2O2 (1:3 vol.) for 12 h; catalyst ink sonicated for 30 min.
ActivationMass loading 0.3 mg cm-2; no thermal activation reported.
Scalability contextLaboratory electrode ink preparation; no scale-up discussed.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherCo-PMDA-2-mbIM catalyst3.59 mgp003 · Electrochemical measurements
AdditiveNafion30 uL · 0.5 wt%p003 · Electrochemical measurements
Solventethanol500 uLp003 · Electrochemical measurements
Solventwater470 uLp003 · Electrochemical measurements
Complete recipeSource: SI

Route 2: Solvothermal

p002 · Preparation of Co-PMDA-2-mbIM

Metal precursorsCoSO4.7H2O, 1.68 mmol
Linker precursors2-methylbenzimidazole (2-mbIM), 3.39 mmol; pyromellitic dianhydride (PMDA), 0.60 mmol
SolventsTHF, 30 mL for metal salt plus 10 mL for ligand dispersion
AtmosphereSealed 50 mL hydrothermal autoclave; atmosphere not otherwise specified
Temperature95
Time48
Work-upWashed several times with methanol and DI water.
ActivationDried in an oven at 60 deg C for 24 h.
Scalability context50 mL autoclave batch; no scale-up discussed.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCoSO4.7H2O1.68 mmolp002 · Preparation of Co-PMDA-2-mbIM
Linker2-methylbenzimidazole [2-mbIM]3.39 mmolp002 · Preparation of Co-PMDA-2-mbIM
Linkerpyromellitic dianhydride [PMDA]0.60 mmolp002 · Preparation of Co-PMDA-2-mbIM
Solventtetrahydrofuran [THF]30 mL + 10 mLp002 · Preparation of Co-PMDA-2-mbIM
Complete recipeSource: SI

Route 3: Drop Cast

p003 · Electrochemical measurements

Solvents500 uL ethanol and 470 uL water
Additives30 uL Nafion (0.5 wt%)
AtmosphereElectrodes used immediately or kept under vacuum before electrochemistry
Temperature25
Substrate orientationCarbon cloth piece, 1 x 3 cm2
Work-upCarbon cloth pretreated with H2SO4:H2O2 (1:3 vol.) for 12 h; catalyst ink sonicated for 30 min.
ActivationMass loading 0.3 mg cm-2.
Scalability contextLaboratory electrode ink preparation; no scale-up discussed.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherCo-PMDA catalyst3.59 mgp003 · Electrochemical measurements
AdditiveNafion30 uL · 0.5 wt%p003 · Electrochemical measurements
Solventethanol500 uLp003 · Electrochemical measurements
Solventwater470 uLp003 · Electrochemical measurements
Complete recipeSource: SI

Route 4: Solvothermal

p002 · Preparation of Co-PMDA

Metal precursorsCoSO4.7H2O, inferred same as Co-PMDA-2-mbIM route
Linker precursorsPMDA, inferred same as Co-PMDA-2-mbIM route; 2-mbIM omitted
SolventsTHF
AtmosphereSealed autoclave; atmosphere not otherwise specified
Temperature95
Time48
Work-upInferred same washing and drying as Co-PMDA-2-mbIM route.
ActivationInferred drying at 60 deg C for 24 h.
Scalability contextNo scale-up discussed.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCoSO4.7H2Oinferred 1.68 mmolp002 · Preparation of Co-PMDA
Linkerpyromellitic dianhydride [PMDA]inferred 0.60 mmolp002 · Preparation of Co-PMDA
Solventtetrahydrofuran [THF]inferred 40 mL totalp002 · Preparation of Co-PMDA