Synthesis evidence

Enhanced bioelectrochemical performance caused by porous metal-organic framework MIL-53(Fe) as the catalyst in microbial fuel cells

Wang H., Jiang L., Chen J. et al. · Process Biochemistry · 2020 · 147-153

2 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 · 2.1. Preparation of MIL-53(Fe) · Fig. 1

Metal precursorsFeCl3.6H2O, 1.35 g
Linker precursors1,4-benzenedicarboxylic acid, 1.66 g
SolventsN,N-dimethylformamide (DMF), source text says 50 mmol
AtmosphereReaction atmosphere not specified; mixture naturally cooled in air to room temperature.
Temperature150
Time12
Work-upSonication to dissolve; transfer to reaction kettle; cool in air; centrifuge; wash several times with DMF and methanol, then wash with distilled water to remove DMF.
ActivationDried at 80 deg C; no separate solvent exchange or activation beyond washing/drying reported.
Scalability contextSmall batch recipe; no yield, autoclave volume or scale-up demonstration reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceFeCl3.6H2O1.35 g2 · 2.1. Preparation of MIL-53(Fe) · Fig. 1
Linker1,4-benzenedicarboxylic acid1.66 g2 · 2.1. Preparation of MIL-53(Fe) · Fig. 1
SolventN,N-dimethylformamide (DMF)50 mmol2 · 2.1. Preparation of MIL-53(Fe) · Fig. 1
Solventmethanol washNot specified2 · 2.1. Preparation of MIL-53(Fe) · Fig. 1
Solventdistilled water washNot specified2 · 2.1. Preparation of MIL-53(Fe) · Fig. 1
Complete recipeSource: Main

Route 2: Drop Cast

2-3 · 2.4. Preparation of MIL-53(Fe) in SS · Fig. 1

Metal precursorsPre-formed MIL-53(Fe) powder; stainless steel (SS)
SolventsAnhydrous ethanol for SS cleaning; deionized water wash
Additives20% PTFE emulsion; 60% PTFE
AtmosphereAir/natural drying; muffle furnace atmosphere not specified
Temperature370
Time0.333
Substrate orientationApplied to both sides of 5 cm2 SS squares; catalyst layer and diffusion layers on opposite sides.
Work-upSS cut into 5 cm2 squares; sonicated in anhydrous ethanol for 10 min; washed with deionized water; dried at 60 deg C; MIL-53(Fe)/PTFE layer applied and dried 30 min; heated at 370 deg C for 20 min and cooled; 60% PTFE applied to other side and heated, repeated to make second and third PTFE layers.
ActivationThermal treatment at 370 deg C for 20 min per layer; no electrochemical activation reported.
Scalability contextElectrode fabrication described on 5 cm2 SS pieces; no larger-area scale-up reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Otherstainless steel (SS)5 cm2 squares2-3 · 2.4. Preparation of MIL-53(Fe) in SS · Fig. 1
OtherMIL-53(Fe)1 mg/cm22-3 · 2.4. Preparation of MIL-53(Fe) in SS · Fig. 1
AdditivePTFE emulsion12 mL · 20%2-3 · 2.4. Preparation of MIL-53(Fe) in SS · Fig. 1
AdditivePTFEmoderate amount · 60%2-3 · 2.4. Preparation of MIL-53(Fe) in SS · Fig. 1
Solventanhydrous ethanolNot specified2-3 · 2.4. Preparation of MIL-53(Fe) in SS · Fig. 1
Solventdeionized waterNot specified2-3 · 2.4. Preparation of MIL-53(Fe) in SS · Fig. 1