cMOF Evidence Base

Synthesis evidence

Generation of Environmentally Persistent Free Radicals on Metal-Organic Frameworks

Ye Y., Li Y., Wang J. et al. · Langmuir · 2022 · 3265-3275

11 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

3266 · Experimental Section - Synthesis of MIL-100(Al)

Metal precursorsAl(NO3)3.9H2O, 0.280 g (0.75 mmol)
Linker precursorstrimethyl 1,3,5-benzenetricarboxylate (Me3BTC), 0.104 g (0.41 mmol)
Solventsdeionised water; DMF; ethanol
Additives0.77 mL of 1 M HNO3 aqueous
AtmosphereTeflon-lined autoclave; vacuum during drying/activation
Temperature210
Time3
Work-upSuspend yellowish product in 40 mL DMF and heat at 150 C for 4 h; filter; Soxhlet extract with water for 12 h; soak in ethanol for 12 h; extract by supercritical CO2; dry under vacuum at 80 C.
ActivationBefore each use, activate under vacuum at 150 C for 12 h.
Scalability contextSmall autoclave batch (25 mL Teflon-lined stainless steel autoclave).
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceAl(NO3)3.9H2O0.280 g (0.75 mmol)3266 · Experimental Section - Synthesis of MIL-100(Al)
LinkerMe3BTC0.104 g (0.41 mmol)3266 · Experimental Section - Synthesis of MIL-100(Al)
Solventdeionized water2.8 mL + 2.8 mL3266 · Experimental Section - Synthesis of MIL-100(Al)
AcidHNO3 aqueous0.77 mL · 1 M3266 · Experimental Section - Synthesis of MIL-100(Al)
SolventDMF40 mL3266 · Experimental Section - Synthesis of MIL-100(Al)
Solventethanolsoaked for 12 h3266 · Experimental Section - Synthesis of MIL-100(Al)
Complete recipeSource: Main

Route 2: Hydrothermal

3266 · Experimental Section - Synthesis of MIL-100(Cr)

Metal precursorsmetallic chromium, 0.104 g (2.00 mmol)
Linker precursorsH3BTC, 0.300 g (1.43 mmol)
Solventswater; deionised water; acetone; ethanol
Additives40% HF, 0.2 mL
AtmosphereTeflon-lined autoclave; vacuum during drying/activation
Temperature220
Time96
Oxidant / reductantmetallic chromium starting reagent
Work-upUltrasound exposure for 30 min; cool; centrifuge; wash three times with deionized water and acetone; soak in ethanol for 12 h; supercritical CO2 extraction; dry under vacuum at 80 C.
ActivationBefore each use, activate under vacuum at 150 C for 12 h.
Scalability context25 mL Teflon-lined autoclave batch.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcemetallic chromium0.104 g (2.00 mmol)3266 · Experimental Section - Synthesis of MIL-100(Cr)
LinkerH3BTC0.300 g (1.43 mmol)3266 · Experimental Section - Synthesis of MIL-100(Cr)
AcidHF0.2 mL · 40%3266 · Experimental Section - Synthesis of MIL-100(Cr)
Solventwater9.6 mL3266 · Experimental Section - Synthesis of MIL-100(Cr)
Partial recipeSource: Main

Route 3: Other

3267 · Experimental Section - EPFR Formation Experiments

Metal precursorsMIL-100(Al) powder
Solventsethanol solution of catechol
Additivescatechol (CT)
AtmosphereAr
Temperature250
Time1
Oxidant / reductantCatechol precursor acts as adsorbate/electron donor during EPFR formation.
Work-upImmerse MIL-100 in ethanol solution of CT for 0.5 h; dry at room temperature; heat CT-exposed framework at 250 C for 1 h under Ar flow of 40 mL min-1.
ActivationParent MIL-100 activated under vacuum at 150 C for 12 h before use.
Scalability contextCatechol concentration and sample mass not reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherMIL-100(Al) materialNot specified3267 · Experimental Section - EPFR Formation Experiments
Othercatechol (CT)ethanol solution, immersion for 0.5 h3267 · Experimental Section - EPFR Formation Experiments
SolventethanolNot specified3267 · Experimental Section - EPFR Formation Experiments
OtherAr40 mL min-13267 · Experimental Section - EPFR Formation Experiments
Partial recipeSource: Main

Route 4: Other

3267 · Experimental Section - EPFR Formation Experiments

Metal precursorsMIL-100(Cr) powder
Solventsethanol solution of catechol
Additivescatechol (CT)
AtmosphereAr
Temperature250
Time1
Oxidant / reductantPhenolic precursor adsorbate.
Work-upSame CT immersion/drying protocol as MIL-100(Al), followed by 250 C thermal treatment under Ar.
ActivationParent MIL-100 activated under vacuum at 150 C for 12 h before use.
Scalability contextCatechol concentration and sample mass not reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherMIL-100(Cr) materialNot specified3267 · Experimental Section - EPFR Formation Experiments
Othercatechol (CT)ethanol solution, immersion for 0.5 h3267 · Experimental Section - EPFR Formation Experiments
SolventethanolNot specified3267 · Experimental Section - EPFR Formation Experiments
OtherAr40 mL min-13267 · Experimental Section - EPFR Formation Experiments
Partial recipeSource: Main

Route 5: Other

3267 · Experimental Section - EPFR Formation Experiments

Metal precursorsMIL-100(Fe) powder
Solventsethanol solution of catechol
Additivescatechol (CT)
AtmosphereAr
Temperature250
Time1
Oxidant / reductantPhenolic precursor adsorbate.
Work-upSame CT immersion/drying protocol as MIL-100(Al), followed by 250 C thermal treatment under Ar.
ActivationParent MIL-100 activated under vacuum at 150 C for 12 h before use.
Scalability contextCatechol concentration and sample mass not reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherMIL-100(Fe) materialNot specified3267 · Experimental Section - EPFR Formation Experiments
Othercatechol (CT)ethanol solution, immersion for 0.5 h3267 · Experimental Section - EPFR Formation Experiments
SolventethanolNot specified3267 · Experimental Section - EPFR Formation Experiments
OtherAr40 mL min-13267 · Experimental Section - EPFR Formation Experiments
Partial recipeSource: Main

Route 6: Other

3267 · Experimental Section - EPFR Formation Experiments

Metal precursorsCT-dosed MIL-100(Al)
SolventsCH2Cl2
Temperature50
Work-upSoxhlet extraction with CH2Cl2 at 50 C to remove unreacted precursor.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
SolventCH2Cl2Not specified3267 · Experimental Section - EPFR Formation Experiments
Complete recipeSource: Main

Route 7: Hydrothermal

3266 · Experimental Section - Synthesis of MIL-100(Fe)

Metal precursorsFeCl3.6H2O, 1.622 g (8.00 mmol)
Linker precursorsH3BTC, 1.387 g (6.60 mmol)
Solventswater; hot ethanol; deionised water; ethanol
AtmosphereTeflon-lined autoclave; vacuum during drying/activation
Temperature130
Time72
Work-upUltrasonic treatment for 30 min; centrifuge after cooling; wash three times with hot ethanol and deionized water; soak in ethanol for 12 h; supercritical CO2 extraction; dry under vacuum at 80 C.
ActivationBefore each use, activate under vacuum at 150 C for 12 h.
Scalability context100 mL Teflon-lined stainless steel autoclave batch.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceFeCl3.6H2O1.622 g (8.00 mmol)3266 · Experimental Section - Synthesis of MIL-100(Fe)
LinkerH3BTC1.387 g (6.60 mmol)3266 · Experimental Section - Synthesis of MIL-100(Fe)
Solventwater50 mL3266 · Experimental Section - Synthesis of MIL-100(Fe)
Solventhot ethanolwashed three times3266 · Experimental Section - Synthesis of MIL-100(Fe)
Partial recipeSource: Main

Route 8: Other

3267 · Experimental Section - EPFR Formation Experiments

Metal precursorsMIL-100(Al) powder
Additives2-chlorophenol (MCP) vapour
AtmosphereAr
Temperature150; 110; 250
Time1; 0.167; 1
Oxidant / reductantPhenolic precursor acts as adsorbate/electron donor during EPFR formation.
Work-upHeat MIL-100 powder at 150 C for 1 h in Ar; inject MCP vapour generated by Ar through MCP pool at 110 C for 10 min; replace MCP vapour with Ar to remove residual unadsorbed precursor; thermally treat at 250 C for 1 h under Ar.
ActivationParent MIL-100 activated under vacuum at 150 C for 12 h before use.
Scalability contextHigh-temperature reaction chamber flow procedure; sample mass not reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMIL-100(Al) powderNot specified3267 · Experimental Section - EPFR Formation Experiments
Other2-chlorophenol (MCP)vapour via MCP pool at 110 C for 10 min3267 · Experimental Section - EPFR Formation Experiments
OtherAr40 mL min-13267 · Experimental Section - EPFR Formation Experiments
Partial recipeSource: Main

Route 9: Other

3267 · Experimental Section - EPFR Formation Experiments

Metal precursorsMIL-100(Cr) powder
Additives2-chlorophenol (MCP) vapour
AtmosphereAr
Temperature150; 110; 250
Time1; 0.167; 1
Oxidant / reductantPhenolic precursor adsorbate.
Work-upSame MCP vapour exposure protocol as MIL-100(Al), followed by 250 C thermal treatment under Ar.
ActivationParent MIL-100 activated under vacuum at 150 C for 12 h before use.
Scalability contextHigh-temperature reaction chamber flow procedure; sample mass not reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMIL-100(Cr) powderNot specified3267 · Experimental Section - EPFR Formation Experiments
Other2-chlorophenol (MCP)vapour via MCP pool at 110 C for 10 min3267 · Experimental Section - EPFR Formation Experiments
OtherAr40 mL min-13267 · Experimental Section - EPFR Formation Experiments
Partial recipeSource: Main

Route 10: Other

3267 · Experimental Section - EPFR Formation Experiments

Metal precursorsMIL-100(Fe) powder
Additives2-chlorophenol (MCP) vapour
AtmosphereAr
Temperature150; 110; 250
Time1; 0.167; 1
Oxidant / reductantPhenolic precursor adsorbate.
Work-upSame MCP vapour exposure protocol as MIL-100(Al), followed by 250 C thermal treatment under Ar.
ActivationParent MIL-100 activated under vacuum at 150 C for 12 h before use.
Scalability contextHigh-temperature reaction chamber flow procedure; sample mass not reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMIL-100(Fe) powderNot specified3267 · Experimental Section - EPFR Formation Experiments
Other2-chlorophenol (MCP)vapour via MCP pool at 110 C for 10 min3267 · Experimental Section - EPFR Formation Experiments
OtherAr40 mL min-13267 · Experimental Section - EPFR Formation Experiments
Partial recipeSource: Main

Route 11: Other

3267 · Experimental Section - EPFR Formation Experiments

Metal precursorsMCP-dosed MIL-100(Al)
SolventsCH2Cl2
Temperature50
Work-upWrap precursor-dosed MIL-100 in filter paper and Soxhlet extract with CH2Cl2 at 50 C to remove unreacted precursors.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
SolventCH2Cl2Not specified3267 · Experimental Section - EPFR Formation Experiments