cMOF Evidence Base

Synthesis evidence

Benign preparation of metal–organic frameworks of trimesic acid and Cu, Co or Ni for potential sensor applications

Sel K., Demirci S., Meydan E. et al. · Journal of Electronic Materials · 2015 · 136-143

3 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

p002-p003 · Synthesis of MOFs in DI Water · Fig. 1

Metal precursorsCoCl2.6H2O; 3.72 x 10^-3 mol Co(II) in 50 mL DI water
Linker precursorsTrimesic acid (TMA), 4.75 x 10^-3 mol in 50 mL DI water
SolventsDI water (18.3 Mohm cm); 50 mL for TMA solution and 50 mL for metal-ion solution
Additives1 M NaOH added dropwise to adjust linker solution to pH 7; HCl listed for metal-ion determination after dissolution
AtmosphereAmbient aqueous room-temperature preparation; atmosphere not otherwise specified
Temperatureroom temperature during precipitation; dried at 70 deg C for 5 h then 100 deg C for 48 h
Time12 h mixing; 5 h drying at 70 deg C; 48 h drying at 100 deg C
Oxidant / reductantNone reported
Work-upMetal-ion solution added dropwise from separator funnel into pH-7 TMA solution in a beaker under 1000 rpm stirring; mixed 12 h; precipitate filtered, washed with excess water and once with ethanol; dried at 70 deg C for 5 h and 100 deg C for 48 h.
ActivationFor N2 adsorption only, MOFs were kept at 50 deg C for 3 days and degassed at 80 deg C for 8 h before analysis.
Scalability contextAqueous, room-temperature dropwise precipitation; no scale-up study reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCoCl2.6H2O3.72 x 10^-3 mol metal ion · in 50 mL DI waterp002-p003 · Synthesis of MOFs in DI Water · Fig. 1
LinkerTrimesic acid (TMA, 99%; Merck)4.75 x 10^-3 mol · in 50 mL DI waterp002-p003 · Synthesis of MOFs in DI Water · Fig. 1
SolventDI water100 mL total reported · 18.3 Mohm cmp002-p003 · Synthesis of MOFs in DI Water · Fig. 1
BaseNaOHdropwise to pH 7 · 1 Mp002-p003 · Synthesis of MOFs in DI Water · Fig. 1
AcidHClused for determination of metal ions after MOF dissolution · 37.5%p002-p003 · Synthesis of MOFs in DI Water · Fig. 1
Complete recipeSource: Main

Route 2: Other

p002-p003 · Synthesis of MOFs in DI Water · Fig. 1

Metal precursorsCuCl2; 3.72 x 10^-3 mol Cu(II) in 50 mL DI water
Linker precursorsTrimesic acid (TMA), 4.75 x 10^-3 mol in 50 mL DI water
SolventsDI water (18.3 Mohm cm); 50 mL for TMA solution and 50 mL for metal-ion solution
Additives1 M NaOH added dropwise to adjust linker solution to pH 7; HCl listed for metal-ion determination after dissolution
AtmosphereAmbient aqueous room-temperature preparation; atmosphere not otherwise specified
Temperatureroom temperature during precipitation; dried at 70 deg C for 5 h then 100 deg C for 48 h
Time12 h mixing; 5 h drying at 70 deg C; 48 h drying at 100 deg C
Oxidant / reductantNone reported
Work-upMetal-ion solution added dropwise from separator funnel into pH-7 TMA solution in a beaker under 1000 rpm stirring; mixed 12 h; precipitate filtered, washed with excess water and once with ethanol; dried at 70 deg C for 5 h and 100 deg C for 48 h.
ActivationFor N2 adsorption only, MOFs were kept at 50 deg C for 3 days and degassed at 80 deg C for 8 h before analysis.
Scalability contextAqueous, room-temperature dropwise precipitation; no scale-up study reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuCl23.72 x 10^-3 mol metal ion · in 50 mL DI waterp002-p003 · Synthesis of MOFs in DI Water · Fig. 1
LinkerTrimesic acid (TMA, 99%; Merck)4.75 x 10^-3 mol · in 50 mL DI waterp002-p003 · Synthesis of MOFs in DI Water · Fig. 1
SolventDI water100 mL total reported · 18.3 Mohm cmp002-p003 · Synthesis of MOFs in DI Water · Fig. 1
BaseNaOHdropwise to pH 7 · 1 Mp002-p003 · Synthesis of MOFs in DI Water · Fig. 1
AcidHClused for determination of metal ions after MOF dissolution · 37.5%p002-p003 · Synthesis of MOFs in DI Water · Fig. 1
Complete recipeSource: Main

Route 3: Other

p002-p003 · Synthesis of MOFs in DI Water · Fig. 1

Metal precursorsNiCl2.6H2O; 3.72 x 10^-3 mol Ni(II) in 50 mL DI water
Linker precursorsTrimesic acid (TMA), 4.75 x 10^-3 mol in 50 mL DI water
SolventsDI water (18.3 Mohm cm); 50 mL for TMA solution and 50 mL for metal-ion solution
Additives1 M NaOH added dropwise to adjust linker solution to pH 7; HCl listed for metal-ion determination after dissolution
AtmosphereAmbient aqueous room-temperature preparation; atmosphere not otherwise specified
Temperatureroom temperature during precipitation; dried at 70 deg C for 5 h then 100 deg C for 48 h
Time12 h mixing; 5 h drying at 70 deg C; 48 h drying at 100 deg C
Oxidant / reductantNone reported
Work-upMetal-ion solution added dropwise from separator funnel into pH-7 TMA solution in a beaker under 1000 rpm stirring; mixed 12 h; precipitate filtered, washed with excess water and once with ethanol; dried at 70 deg C for 5 h and 100 deg C for 48 h.
ActivationFor N2 adsorption only, MOFs were kept at 50 deg C for 3 days and degassed at 80 deg C for 8 h before analysis.
Scalability contextAqueous, room-temperature dropwise precipitation; no scale-up study reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2O3.72 x 10^-3 mol metal ion · in 50 mL DI waterp002-p003 · Synthesis of MOFs in DI Water · Fig. 1
LinkerTrimesic acid (TMA, 99%; Merck)4.75 x 10^-3 mol · in 50 mL DI waterp002-p003 · Synthesis of MOFs in DI Water · Fig. 1
SolventDI water100 mL total reported · 18.3 Mohm cmp002-p003 · Synthesis of MOFs in DI Water · Fig. 1
BaseNaOHdropwise to pH 7 · 1 Mp002-p003 · Synthesis of MOFs in DI Water · Fig. 1
AcidHClused for determination of metal ions after MOF dissolution · 37.5%p002-p003 · Synthesis of MOFs in DI Water · Fig. 1