Synthesis evidence

Ionic liquid supported nickel-based metal-organic framework for electrochemical sensing of hydrogen peroxide and electrocatalytic oxidation of methanol

Wang N., Liang S., Zhang L. et al. · Colloids and Surfaces A: Physicochemical and Engineering Aspects · 2020 · 125199

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: Drop Cast

2 · 2.4. Fabrication of the Ni-MOF modified electrode

Metal precursorspre-synthesised Ni-MOF
Solventsethanol suspension; nitric acid/water, water and ethanol used for electrode cleaning
AdditivesNafion (1 wt%)
Atmosphereambient, not otherwise stated
Substrate orientationglassy carbon electrode, 5 mm diameter
Work-upGCE polished with 1.0, 0.3 and 0.05 um alumina; sonicated in nitric acid/water, ultrapure water and ethanol for 5 min each; Ni-MOF suspension and Nafion dripped onto GCE.
ActivationDried under an infrared lamp.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
OtherNi-MOF material5 mg dispersed in 1 mL ethanol; 10 uL suspension applied · 5 mg/mL2 · 2.4. Fabrication of the Ni-MOF modified electrode
Solventethanol1 mL for Ni-MOF suspension2 · 2.4. Fabrication of the Ni-MOF modified electrode
AdditiveNafion5 uL · 1 wt%2 · 2.4. Fabrication of the Ni-MOF modified electrode
Acidnitric acid/watersonication for 5 min · about 1:1 volume ratio2 · 2.4. Fabrication of the Ni-MOF modified electrode
Otherglassy carbon electrodediameter 5 mm2 · 2.4. Fabrication of the Ni-MOF modified electrode
Complete recipeSource: Main

Route 2: Other

2 · 2.3. Synthesis of the Ni-MOF

Metal precursorsNi(OAc)2.4H2O (0.5 mmol)
Linker precursorsH3BTC (0.5 mmol); [EMI]Br also acts as ligand
Solvents1.0 mL [EMI]Br ionic liquid
Additives[EMI]Br ionic liquid
Atmospherenot stated
Temperature180
Time72
Work-upNaturally cooled; solid product washed several times with DMF and ethanol.
ActivationDried at 60 C overnight in a vacuum oven.
Scalability contextAutoclave ionothermal synthesis in a 25 mL PTFE-lined stainless-steel vessel; no scale-up data reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNickel acetate (Ni(OAc)2.4H2O)0.5 mmol2 · 2.3. Synthesis of the Ni-MOF
Linker1,3,5-benzenetricarboxylic acid (H3BTC)0.5 mmol2 · 2.3. Synthesis of the Ni-MOF
Solvent1-ethyl-3-methylimidazolium bromide ([EMI]Br, 98%)1.0 mL2 · 2.3. Synthesis of the Ni-MOF
Additive1-ethyl-3-methylimidazolium bromide ([EMI]Br)1.0 mL2 · 2.3. Synthesis of the Ni-MOF
SolventDMFwashed several times2 · 2.3. Synthesis of the Ni-MOF
Solventethanolwashed several times2 · 2.3. Synthesis of the Ni-MOF