cMOF Evidence Base

Synthesis evidence

Understanding Solvothermal Growth of Metal-Organic Framework Colloids for CO2Capture Applications

Hsieh P.-F., Law Z.X., Lin C.-H. et al. · Langmuir · 2022 · 4415-4424

18 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Solvothermal

4416-4417 · Materials and Methods · Table 1

Metal precursorscopper(II) nitrate trihydrate; main recipe states 0.2319 g Cu precursor for the baseline recipe
Linker precursors1,3,5-benzenetricarboxylic acid (H3BTC), target CBTC=0.021 mol/L
Solventsethanol, 30 mL
Additivespolyvinylpyrrolidone (PVP, average molecular mass 10000 Da), 0.24 g stabiliser; nitric acid used only for ES-DMA dilution/pH adjustment
Atmospheresealed 50 mL Teflon-lined stainless-steel autoclave; gas atmosphere not specified
Temperature100
Time8
Work-upUnreacted/unbound ligands, metal ions and surfactants washed with ethanol about 3 times by cyclic vacuum filtration.
ActivationOvernight drying at 120 deg C, described as activation of the MOF; BET samples additionally degassed at 120 deg C for at least 8 h; CO2 pulse samples degassed under He at 120 deg C for 30 min.
Scalability contextPrepared as 30 mL solvothermal batches in 50 mL autoclaves.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper(II) nitrate trihydrate0.2319 g for baseline recipe · not individually stated4416-4417 · Materials and Methods · Table 1
Linker1,3,5-benzenetricarboxylic acid (H3BTC)not printed for this varied-CBTC sample · CBTC = 0.021 mol/L4416-4417 · Materials and Methods · Table 1
AdditivePolyvinylpyrrolidone (PVP, average molecular mass 10000 Da)0.24 g4416-4417 · Materials and Methods · Table 1
Solventethanol30 mL · >=99.8%4416-4417 · Materials and Methods · Table 1
Complete recipeSource: Main

Route 2: Solvothermal

4416-4417 · Materials and Methods · Table 1

Metal precursorscopper(II) nitrate trihydrate; main recipe states 0.2319 g Cu precursor for the baseline recipe
Linker precursors1,3,5-benzenetricarboxylic acid (H3BTC), target CBTC=0.064 mol/L
Solventsethanol, 30 mL
Additivespolyvinylpyrrolidone (PVP, average molecular mass 10000 Da), 0.24 g stabiliser; nitric acid used only for ES-DMA dilution/pH adjustment
Atmospheresealed 50 mL Teflon-lined stainless-steel autoclave; gas atmosphere not specified
Temperature100
Time14
Work-upUnreacted/unbound ligands, metal ions and surfactants washed with ethanol about 3 times by cyclic vacuum filtration.
ActivationOvernight drying at 120 deg C, described as activation of the MOF; BET samples additionally degassed at 120 deg C for at least 8 h; CO2 pulse samples degassed under He at 120 deg C for 30 min.
Scalability contextPrepared as 30 mL solvothermal batches in 50 mL autoclaves.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper(II) nitrate trihydrate0.2319 g for baseline recipe · not individually stated4416-4417 · Materials and Methods · Table 1
Linker1,3,5-benzenetricarboxylic acid (H3BTC)0.2017 g for baseline recipe · CBTC = 0.064 mol/L4416-4417 · Materials and Methods · Table 1
AdditivePolyvinylpyrrolidone (PVP, average molecular mass 10000 Da)0.24 g4416-4417 · Materials and Methods · Table 1
Solventethanol30 mL · >=99.8%4416-4417 · Materials and Methods · Table 1
Complete recipeSource: Main

Route 3: Solvothermal

4416-4417 · Materials and Methods · Table 1

Metal precursorscopper(II) nitrate trihydrate; main recipe states 0.2319 g Cu precursor for the baseline recipe
Linker precursors1,3,5-benzenetricarboxylic acid (H3BTC), target CBTC=0.064 mol/L
Solventsethanol, 30 mL
Additivespolyvinylpyrrolidone (PVP, average molecular mass 10000 Da), 0.24 g stabiliser; nitric acid used only for ES-DMA dilution/pH adjustment
Atmospheresealed 50 mL Teflon-lined stainless-steel autoclave; gas atmosphere not specified
Temperature100
Time20
Work-upUnreacted/unbound ligands, metal ions and surfactants washed with ethanol about 3 times by cyclic vacuum filtration.
ActivationOvernight drying at 120 deg C, described as activation of the MOF; BET samples additionally degassed at 120 deg C for at least 8 h; CO2 pulse samples degassed under He at 120 deg C for 30 min.
Scalability contextPrepared as 30 mL solvothermal batches in 50 mL autoclaves.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper(II) nitrate trihydrate0.2319 g for baseline recipe · not individually stated4416-4417 · Materials and Methods · Table 1
Linker1,3,5-benzenetricarboxylic acid (H3BTC)0.2017 g for baseline recipe · CBTC = 0.064 mol/L4416-4417 · Materials and Methods · Table 1
AdditivePolyvinylpyrrolidone (PVP, average molecular mass 10000 Da)0.24 g4416-4417 · Materials and Methods · Table 1
Solventethanol30 mL · >=99.8%4416-4417 · Materials and Methods · Table 1
Complete recipeSource: Main

Route 4: Solvothermal

4416-4417 · Materials and Methods · Table 1

Metal precursorscopper(II) nitrate trihydrate; main recipe states 0.2319 g Cu precursor for the baseline recipe
Linker precursors1,3,5-benzenetricarboxylic acid (H3BTC), target CBTC=0.064 mol/L
Solventsethanol, 30 mL
Additivespolyvinylpyrrolidone (PVP, average molecular mass 10000 Da), 0.24 g stabiliser; nitric acid used only for ES-DMA dilution/pH adjustment
Atmospheresealed 50 mL Teflon-lined stainless-steel autoclave; gas atmosphere not specified
Temperature100
Time3
Work-upUnreacted/unbound ligands, metal ions and surfactants washed with ethanol about 3 times by cyclic vacuum filtration.
ActivationOvernight drying at 120 deg C, described as activation of the MOF; BET samples additionally degassed at 120 deg C for at least 8 h; CO2 pulse samples degassed under He at 120 deg C for 30 min.
Scalability contextPrepared as 30 mL solvothermal batches in 50 mL autoclaves.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper(II) nitrate trihydrate0.2319 g for baseline recipe · not individually stated4416-4417 · Materials and Methods · Table 1
Linker1,3,5-benzenetricarboxylic acid (H3BTC)0.2017 g for baseline recipe · CBTC = 0.064 mol/L4416-4417 · Materials and Methods · Table 1
AdditivePolyvinylpyrrolidone (PVP, average molecular mass 10000 Da)0.24 g4416-4417 · Materials and Methods · Table 1
Solventethanol30 mL · >=99.8%4416-4417 · Materials and Methods · Table 1
Complete recipeSource: Main

Route 5: Solvothermal

4416-4417 · Materials and Methods · Table 1

Metal precursorscopper(II) nitrate trihydrate; main recipe states 0.2319 g Cu precursor for the baseline recipe
Linker precursors1,3,5-benzenetricarboxylic acid (H3BTC), target CBTC=0.064 mol/L
Solventsethanol, 30 mL
Additivespolyvinylpyrrolidone (PVP, average molecular mass 10000 Da), 0.24 g stabiliser; nitric acid used only for ES-DMA dilution/pH adjustment
Atmospheresealed 50 mL Teflon-lined stainless-steel autoclave; gas atmosphere not specified
Temperature100
Time5
Work-upUnreacted/unbound ligands, metal ions and surfactants washed with ethanol about 3 times by cyclic vacuum filtration.
ActivationOvernight drying at 120 deg C, described as activation of the MOF; BET samples additionally degassed at 120 deg C for at least 8 h; CO2 pulse samples degassed under He at 120 deg C for 30 min.
Scalability contextPrepared as 30 mL solvothermal batches in 50 mL autoclaves.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper(II) nitrate trihydrate0.2319 g for baseline recipe · not individually stated4416-4417 · Materials and Methods · Table 1
Linker1,3,5-benzenetricarboxylic acid (H3BTC)0.2017 g for baseline recipe · CBTC = 0.064 mol/L4416-4417 · Materials and Methods · Table 1
AdditivePolyvinylpyrrolidone (PVP, average molecular mass 10000 Da)0.24 g4416-4417 · Materials and Methods · Table 1
Solventethanol30 mL · >=99.8%4416-4417 · Materials and Methods · Table 1
Complete recipeSource: Main

Route 6: Solvothermal

4416-4417 · Materials and Methods · Table 1

Metal precursorscopper(II) nitrate trihydrate; main recipe states 0.2319 g Cu precursor for the baseline recipe
Linker precursors1,3,5-benzenetricarboxylic acid (H3BTC), target CBTC=0.064 mol/L
Solventsethanol, 30 mL
Additivespolyvinylpyrrolidone (PVP, average molecular mass 10000 Da), 0.24 g stabiliser; nitric acid used only for ES-DMA dilution/pH adjustment
Atmospheresealed 50 mL Teflon-lined stainless-steel autoclave; gas atmosphere not specified
Temperature100
Time8
Work-upUnreacted/unbound ligands, metal ions and surfactants washed with ethanol about 3 times by cyclic vacuum filtration.
ActivationOvernight drying at 120 deg C, described as activation of the MOF; BET samples additionally degassed at 120 deg C for at least 8 h; CO2 pulse samples degassed under He at 120 deg C for 30 min.
Scalability contextPrepared as 30 mL solvothermal batches in 50 mL autoclaves.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper(II) nitrate trihydrate0.2319 g for baseline recipe · not individually stated4416-4417 · Materials and Methods · Table 1
Linker1,3,5-benzenetricarboxylic acid (H3BTC)0.2017 g for baseline recipe · CBTC = 0.064 mol/L4416-4417 · Materials and Methods · Table 1
AdditivePolyvinylpyrrolidone (PVP, average molecular mass 10000 Da)0.24 g4416-4417 · Materials and Methods · Table 1
Solventethanol30 mL · >=99.8%4416-4417 · Materials and Methods · Table 1
Complete recipeSource: Main

Route 7: Solvothermal

4416-4417 · Materials and Methods · Table 1

Metal precursorscopper(II) nitrate trihydrate; main recipe states 0.2319 g Cu precursor for the baseline recipe
Linker precursors1,3,5-benzenetricarboxylic acid (H3BTC), target CBTC=0.064 mol/L
Solventsethanol, 30 mL
Additivespolyvinylpyrrolidone (PVP, average molecular mass 10000 Da), 0.24 g stabiliser; nitric acid used only for ES-DMA dilution/pH adjustment
Atmospheresealed 50 mL Teflon-lined stainless-steel autoclave; gas atmosphere not specified
Temperature120
Time14
Work-upUnreacted/unbound ligands, metal ions and surfactants washed with ethanol about 3 times by cyclic vacuum filtration.
ActivationOvernight drying at 120 deg C, described as activation of the MOF; BET samples additionally degassed at 120 deg C for at least 8 h; CO2 pulse samples degassed under He at 120 deg C for 30 min.
Scalability contextPrepared as 30 mL solvothermal batches in 50 mL autoclaves.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper(II) nitrate trihydrate0.2319 g for baseline recipe · not individually stated4416-4417 · Materials and Methods · Table 1
Linker1,3,5-benzenetricarboxylic acid (H3BTC)0.2017 g for baseline recipe · CBTC = 0.064 mol/L4416-4417 · Materials and Methods · Table 1
AdditivePolyvinylpyrrolidone (PVP, average molecular mass 10000 Da)0.24 g4416-4417 · Materials and Methods · Table 1
Solventethanol30 mL · >=99.8%4416-4417 · Materials and Methods · Table 1
Complete recipeSource: Main

Route 8: Solvothermal

4416-4417 · Materials and Methods · Table 1

Metal precursorscopper(II) nitrate trihydrate; main recipe states 0.2319 g Cu precursor for the baseline recipe
Linker precursors1,3,5-benzenetricarboxylic acid (H3BTC), target CBTC=0.064 mol/L
Solventsethanol, 30 mL
Additivespolyvinylpyrrolidone (PVP, average molecular mass 10000 Da), 0.24 g stabiliser; nitric acid used only for ES-DMA dilution/pH adjustment
Atmospheresealed 50 mL Teflon-lined stainless-steel autoclave; gas atmosphere not specified
Temperature120
Time20
Work-upUnreacted/unbound ligands, metal ions and surfactants washed with ethanol about 3 times by cyclic vacuum filtration.
ActivationOvernight drying at 120 deg C, described as activation of the MOF; BET samples additionally degassed at 120 deg C for at least 8 h; CO2 pulse samples degassed under He at 120 deg C for 30 min.
Scalability contextPrepared as 30 mL solvothermal batches in 50 mL autoclaves.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper(II) nitrate trihydrate0.2319 g for baseline recipe · not individually stated4416-4417 · Materials and Methods · Table 1
Linker1,3,5-benzenetricarboxylic acid (H3BTC)0.2017 g for baseline recipe · CBTC = 0.064 mol/L4416-4417 · Materials and Methods · Table 1
AdditivePolyvinylpyrrolidone (PVP, average molecular mass 10000 Da)0.24 g4416-4417 · Materials and Methods · Table 1
Solventethanol30 mL · >=99.8%4416-4417 · Materials and Methods · Table 1
Complete recipeSource: Main

Route 9: Solvothermal

4416-4417 · Materials and Methods · Table 1

Metal precursorscopper(II) nitrate trihydrate; main recipe states 0.2319 g Cu precursor for the baseline recipe
Linker precursors1,3,5-benzenetricarboxylic acid (H3BTC), target CBTC=0.064 mol/L
Solventsethanol, 30 mL
Additivespolyvinylpyrrolidone (PVP, average molecular mass 10000 Da), 0.24 g stabiliser; nitric acid used only for ES-DMA dilution/pH adjustment
Atmospheresealed 50 mL Teflon-lined stainless-steel autoclave; gas atmosphere not specified
Temperature120
Time3
Work-upUnreacted/unbound ligands, metal ions and surfactants washed with ethanol about 3 times by cyclic vacuum filtration.
ActivationOvernight drying at 120 deg C, described as activation of the MOF; BET samples additionally degassed at 120 deg C for at least 8 h; CO2 pulse samples degassed under He at 120 deg C for 30 min.
Scalability contextPrepared as 30 mL solvothermal batches in 50 mL autoclaves.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper(II) nitrate trihydrate0.2319 g for baseline recipe · not individually stated4416-4417 · Materials and Methods · Table 1
Linker1,3,5-benzenetricarboxylic acid (H3BTC)0.2017 g for baseline recipe · CBTC = 0.064 mol/L4416-4417 · Materials and Methods · Table 1
AdditivePolyvinylpyrrolidone (PVP, average molecular mass 10000 Da)0.24 g4416-4417 · Materials and Methods · Table 1
Solventethanol30 mL · >=99.8%4416-4417 · Materials and Methods · Table 1
Complete recipeSource: Main

Route 10: Solvothermal

4416-4417 · Materials and Methods · Table 1

Metal precursorscopper(II) nitrate trihydrate; main recipe states 0.2319 g Cu precursor for the baseline recipe
Linker precursors1,3,5-benzenetricarboxylic acid (H3BTC), target CBTC=0.064 mol/L
Solventsethanol, 30 mL
Additivespolyvinylpyrrolidone (PVP, average molecular mass 10000 Da), 0.24 g stabiliser; nitric acid used only for ES-DMA dilution/pH adjustment
Atmospheresealed 50 mL Teflon-lined stainless-steel autoclave; gas atmosphere not specified
Temperature120
Time5
Work-upUnreacted/unbound ligands, metal ions and surfactants washed with ethanol about 3 times by cyclic vacuum filtration.
ActivationOvernight drying at 120 deg C, described as activation of the MOF; BET samples additionally degassed at 120 deg C for at least 8 h; CO2 pulse samples degassed under He at 120 deg C for 30 min.
Scalability contextPrepared as 30 mL solvothermal batches in 50 mL autoclaves.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper(II) nitrate trihydrate0.2319 g for baseline recipe · not individually stated4416-4417 · Materials and Methods · Table 1
Linker1,3,5-benzenetricarboxylic acid (H3BTC)0.2017 g for baseline recipe · CBTC = 0.064 mol/L4416-4417 · Materials and Methods · Table 1
AdditivePolyvinylpyrrolidone (PVP, average molecular mass 10000 Da)0.24 g4416-4417 · Materials and Methods · Table 1
Solventethanol30 mL · >=99.8%4416-4417 · Materials and Methods · Table 1
Complete recipeSource: Main

Route 11: Solvothermal

4416-4417 · Materials and Methods · Table 1

Metal precursorscopper(II) nitrate trihydrate; main recipe states 0.2319 g Cu precursor for the baseline recipe
Linker precursors1,3,5-benzenetricarboxylic acid (H3BTC), target CBTC=0.064 mol/L
Solventsethanol, 30 mL
Additivespolyvinylpyrrolidone (PVP, average molecular mass 10000 Da), 0.24 g stabiliser; nitric acid used only for ES-DMA dilution/pH adjustment
Atmospheresealed 50 mL Teflon-lined stainless-steel autoclave; gas atmosphere not specified
Temperature120
Time8
Work-upUnreacted/unbound ligands, metal ions and surfactants washed with ethanol about 3 times by cyclic vacuum filtration.
ActivationOvernight drying at 120 deg C, described as activation of the MOF; BET samples additionally degassed at 120 deg C for at least 8 h; CO2 pulse samples degassed under He at 120 deg C for 30 min.
Scalability contextPrepared as 30 mL solvothermal batches in 50 mL autoclaves.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper(II) nitrate trihydrate0.2319 g for baseline recipe · not individually stated4416-4417 · Materials and Methods · Table 1
Linker1,3,5-benzenetricarboxylic acid (H3BTC)0.2017 g for baseline recipe · CBTC = 0.064 mol/L4416-4417 · Materials and Methods · Table 1
AdditivePolyvinylpyrrolidone (PVP, average molecular mass 10000 Da)0.24 g4416-4417 · Materials and Methods · Table 1
Solventethanol30 mL · >=99.8%4416-4417 · Materials and Methods · Table 1
Complete recipeSource: Main

Route 12: Solvothermal

4416-4417 · Materials and Methods · Table 1

Metal precursorscopper(II) nitrate trihydrate; main recipe states 0.2319 g Cu precursor for the baseline recipe
Linker precursors1,3,5-benzenetricarboxylic acid (H3BTC), target CBTC=0.064 mol/L
Solventsethanol, 30 mL
Additivespolyvinylpyrrolidone (PVP, average molecular mass 10000 Da), 0.24 g stabiliser; nitric acid used only for ES-DMA dilution/pH adjustment
Atmospheresealed 50 mL Teflon-lined stainless-steel autoclave; gas atmosphere not specified
Temperature80
Time14
Work-upUnreacted/unbound ligands, metal ions and surfactants washed with ethanol about 3 times by cyclic vacuum filtration.
ActivationOvernight drying at 120 deg C, described as activation of the MOF; BET samples additionally degassed at 120 deg C for at least 8 h; CO2 pulse samples degassed under He at 120 deg C for 30 min.
Scalability contextPrepared as 30 mL solvothermal batches in 50 mL autoclaves.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper(II) nitrate trihydrate0.2319 g for baseline recipe · not individually stated4416-4417 · Materials and Methods · Table 1
Linker1,3,5-benzenetricarboxylic acid (H3BTC)0.2017 g for baseline recipe · CBTC = 0.064 mol/L4416-4417 · Materials and Methods · Table 1
AdditivePolyvinylpyrrolidone (PVP, average molecular mass 10000 Da)0.24 g4416-4417 · Materials and Methods · Table 1
Solventethanol30 mL · >=99.8%4416-4417 · Materials and Methods · Table 1
Complete recipeSource: Main

Route 13: Solvothermal

4416-4417 · Materials and Methods · Table 1

Metal precursorscopper(II) nitrate trihydrate; main recipe states 0.2319 g Cu precursor for the baseline recipe
Linker precursors1,3,5-benzenetricarboxylic acid (H3BTC), target CBTC=0.064 mol/L
Solventsethanol, 30 mL
Additivespolyvinylpyrrolidone (PVP, average molecular mass 10000 Da), 0.24 g stabiliser; nitric acid used only for ES-DMA dilution/pH adjustment
Atmospheresealed 50 mL Teflon-lined stainless-steel autoclave; gas atmosphere not specified
Temperature80
Time20
Work-upUnreacted/unbound ligands, metal ions and surfactants washed with ethanol about 3 times by cyclic vacuum filtration.
ActivationOvernight drying at 120 deg C, described as activation of the MOF; BET samples additionally degassed at 120 deg C for at least 8 h; CO2 pulse samples degassed under He at 120 deg C for 30 min.
Scalability contextPrepared as 30 mL solvothermal batches in 50 mL autoclaves.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper(II) nitrate trihydrate0.2319 g for baseline recipe · not individually stated4416-4417 · Materials and Methods · Table 1
Linker1,3,5-benzenetricarboxylic acid (H3BTC)0.2017 g for baseline recipe · CBTC = 0.064 mol/L4416-4417 · Materials and Methods · Table 1
AdditivePolyvinylpyrrolidone (PVP, average molecular mass 10000 Da)0.24 g4416-4417 · Materials and Methods · Table 1
Solventethanol30 mL · >=99.8%4416-4417 · Materials and Methods · Table 1
Complete recipeSource: Main

Route 14: Solvothermal

4416-4417 · Materials and Methods · Table 1

Metal precursorscopper(II) nitrate trihydrate; main recipe states 0.2319 g Cu precursor for the baseline recipe
Linker precursors1,3,5-benzenetricarboxylic acid (H3BTC), target CBTC=0.064 mol/L
Solventsethanol, 30 mL
Additivespolyvinylpyrrolidone (PVP, average molecular mass 10000 Da), 0.24 g stabiliser; nitric acid used only for ES-DMA dilution/pH adjustment
Atmospheresealed 50 mL Teflon-lined stainless-steel autoclave; gas atmosphere not specified
Temperature80
Time3
Work-upUnreacted/unbound ligands, metal ions and surfactants washed with ethanol about 3 times by cyclic vacuum filtration.
ActivationOvernight drying at 120 deg C, described as activation of the MOF; BET samples additionally degassed at 120 deg C for at least 8 h; CO2 pulse samples degassed under He at 120 deg C for 30 min.
Scalability contextPrepared as 30 mL solvothermal batches in 50 mL autoclaves.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper(II) nitrate trihydrate0.2319 g for baseline recipe · not individually stated4416-4417 · Materials and Methods · Table 1
Linker1,3,5-benzenetricarboxylic acid (H3BTC)0.2017 g for baseline recipe · CBTC = 0.064 mol/L4416-4417 · Materials and Methods · Table 1
AdditivePolyvinylpyrrolidone (PVP, average molecular mass 10000 Da)0.24 g4416-4417 · Materials and Methods · Table 1
Solventethanol30 mL · >=99.8%4416-4417 · Materials and Methods · Table 1
Complete recipeSource: Main

Route 15: Solvothermal

4416-4417 · Materials and Methods · Table 1

Metal precursorscopper(II) nitrate trihydrate; main recipe states 0.2319 g Cu precursor for the baseline recipe
Linker precursors1,3,5-benzenetricarboxylic acid (H3BTC), target CBTC=0.064 mol/L
Solventsethanol, 30 mL
Additivespolyvinylpyrrolidone (PVP, average molecular mass 10000 Da), 0.24 g stabiliser; nitric acid used only for ES-DMA dilution/pH adjustment
Atmospheresealed 50 mL Teflon-lined stainless-steel autoclave; gas atmosphere not specified
Temperature80
Time5
Work-upUnreacted/unbound ligands, metal ions and surfactants washed with ethanol about 3 times by cyclic vacuum filtration.
ActivationOvernight drying at 120 deg C, described as activation of the MOF; BET samples additionally degassed at 120 deg C for at least 8 h; CO2 pulse samples degassed under He at 120 deg C for 30 min.
Scalability contextPrepared as 30 mL solvothermal batches in 50 mL autoclaves.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper(II) nitrate trihydrate0.2319 g for baseline recipe · not individually stated4416-4417 · Materials and Methods · Table 1
Linker1,3,5-benzenetricarboxylic acid (H3BTC)0.2017 g for baseline recipe · CBTC = 0.064 mol/L4416-4417 · Materials and Methods · Table 1
AdditivePolyvinylpyrrolidone (PVP, average molecular mass 10000 Da)0.24 g4416-4417 · Materials and Methods · Table 1
Solventethanol30 mL · >=99.8%4416-4417 · Materials and Methods · Table 1
Complete recipeSource: Main

Route 16: Solvothermal

4416-4417 · Materials and Methods · Table 1

Metal precursorscopper(II) nitrate trihydrate; main recipe states 0.2319 g Cu precursor for the baseline recipe
Linker precursors1,3,5-benzenetricarboxylic acid (H3BTC), target CBTC=0.064 mol/L
Solventsethanol, 30 mL
Additivespolyvinylpyrrolidone (PVP, average molecular mass 10000 Da), 0.24 g stabiliser; nitric acid used only for ES-DMA dilution/pH adjustment
Atmospheresealed 50 mL Teflon-lined stainless-steel autoclave; gas atmosphere not specified
Temperature80
Time8
Work-upUnreacted/unbound ligands, metal ions and surfactants washed with ethanol about 3 times by cyclic vacuum filtration.
ActivationOvernight drying at 120 deg C, described as activation of the MOF; BET samples additionally degassed at 120 deg C for at least 8 h; CO2 pulse samples degassed under He at 120 deg C for 30 min.
Scalability contextPrepared as 30 mL solvothermal batches in 50 mL autoclaves.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper(II) nitrate trihydrate0.2319 g for baseline recipe · not individually stated4416-4417 · Materials and Methods · Table 1
Linker1,3,5-benzenetricarboxylic acid (H3BTC)0.2017 g for baseline recipe · CBTC = 0.064 mol/L4416-4417 · Materials and Methods · Table 1
AdditivePolyvinylpyrrolidone (PVP, average molecular mass 10000 Da)0.24 g4416-4417 · Materials and Methods · Table 1
Solventethanol30 mL · >=99.8%4416-4417 · Materials and Methods · Table 1
Partial recipeSource: Main

Route 17: Solvothermal

4416-4417 · Materials and Methods · Table 1

Metal precursorscopper(II) nitrate trihydrate; main recipe states 0.2319 g Cu precursor for the baseline recipe
Linker precursors1,3,5-benzenetricarboxylic acid (H3BTC), target CBTC=0.192 mol/L
Solventsethanol, 30 mL
Additivespolyvinylpyrrolidone (PVP, average molecular mass 10000 Da), 0.24 g stabiliser; nitric acid used only for ES-DMA dilution/pH adjustment
Atmospheresealed 50 mL Teflon-lined stainless-steel autoclave; gas atmosphere not specified
Temperature100
Time8
Work-upUnreacted/unbound ligands, metal ions and surfactants washed with ethanol about 3 times by cyclic vacuum filtration.
ActivationOvernight drying at 120 deg C, described as activation of the MOF; BET samples additionally degassed at 120 deg C for at least 8 h; CO2 pulse samples degassed under He at 120 deg C for 30 min.
Scalability contextPrepared as 30 mL solvothermal batches in 50 mL autoclaves.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper(II) nitrate trihydrate0.2319 g for baseline recipe · not individually stated4416-4417 · Materials and Methods · Table 1
Linker1,3,5-benzenetricarboxylic acid (H3BTC)not printed for this varied-CBTC sample · CBTC = 0.192 mol/L4416-4417 · Materials and Methods · Table 1
AdditivePolyvinylpyrrolidone (PVP, average molecular mass 10000 Da)0.24 g4416-4417 · Materials and Methods · Table 1
Solventethanol30 mL · >=99.8%4416-4417 · Materials and Methods · Table 1
Partial recipeSource: SI

Route 18: Solvothermal

S16 · Material characterization of the Cu-MOF prepared by a different amount of copper · Figure S13

Metal precursorscopper(II) nitrate trihydrate; copper-source concentration CCu=0.192 mol/L, a three-fold increase of CCu
Linker precursors1,3,5-benzenetricarboxylic acid (H3BTC), CBTC=0.064 mol/L
Solventsethanol; volume not restated in SI Section 7, presumed same solvothermal system as main recipe
AdditivesPVP stabiliser used for Cu-MOF colloids in main method; exact amount not restated for this SI-only variant
Atmospheresealed solvothermal autoclave presumed; atmosphere not restated in SI
Temperature100
Time8
Work-upnot restated in SI Section 7; main route washes Cu-MOF colloids with ethanol by cyclic vacuum filtration
Activationnot restated in SI Section 7; main route dries/activates overnight at 120 deg C
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper source, identified in main method as copper(II) nitrate trihydratenot printed for SI variant · CCu = 0.192 mol/LS16 · Material characterization of the Cu-MOF prepared by a different amount of copper · Figure S13
LinkerH3BTCnot restated · CBTC = 0.064 mol/LS16 · Material characterization of the Cu-MOF prepared by a different amount of copper · Figure S13
AdditivePVP stabilisernot restatedS16 · Material characterization of the Cu-MOF prepared by a different amount of copper · Figure S13
Solventethanolnot restatedS16 · Material characterization of the Cu-MOF prepared by a different amount of copper · Figure S13