Patent
Atlas literature
Patent
US 8,871,171Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 2. Atomic force microscopy (AFM) data of graphene sheets produced by M WI of 5 s oli d graphite oxide.
Figure 3A-F. X-ray diffraction (XRD) patterns of GO containing 2% metal precursors before and after the MWI of the solid. A, silver; B, cobalt; C, copper; D, iron; E, nickel; F, palladium.
Figure 4. XRD patterns of GO containing 5% metal precursors A, before and B, after the 10 MWI of the solid.
Figure 5. Photographs of solid graphite oxide containing metal salts before (top) and after (bottom) microwave irradiation (M W I) of the solid.
Figure 6A-C. TEM images of graphene sheets containing 2% (wt) Pd Nanoparticles produced by MWI of solid graphite oxide containing 2% (wt) palladium nitrate. A, 15 1 pm scale; B, 200 nm scale; C, 100 nm scale.
Figure 7A and B. (a) Small-angle XRD patterns of graphite, GO, graphene, and Pd/graphene (Pd/G) samples. (b) Small-angle XRD pattern of Pd/graphite oxide (Pd/GO) prepared by MWI of a mixture of GO and Pd nitrate solution in water without the addition of hydrazine hydrate. 20
Figure 8 A and B. (a) Raman spectra of the graphene and Pd/G samples prepared by the hydrazine hydrate (HH) MWI method in the G- and D-regions and (b) in the 2D-region.
Figure 9A and B. (a) SEM image and (b) EDS analysis of Pd/G prepared by the HH-MWI method.
Figure 10 A and B. TEM images of (a) 7.9 wt.% Pd/G and (b) 6.4 wt.% Pd/GO prepared by 25 MWI of a mixture of graphite oxide (GO) and palladium nitrate in the presence and absence of hydrazine hydrate, respectively.
Figure 11 A and B. A, Comparison of the TGA plots of graphite oxide (GO), graphene (G), and Pd/GO and Pd/G catalysts; B, Scheme of Suzuki cross-coupling reaction w ith Pd/G and Pd/GO. 30
Figure 1 2. Effect of catalyst concentrations for the Pd/G and Pd/GO on the conversion of reaction (
Figure 11 B).
Figure 13A andB. TEM images of (a) Pd/G after the 10th run and (b) Pd/GO after the 7th -4- WO 2011/119961 PCT/US₂ 01 1/029998 run.
Figure 14. XPS spectra of the Pd 3d5/2 and 3d3/2 electrons' binding energies for Pd/G and Pd/GO catalysts before and after Suzuki reactions.
Figure 15. Evaluation of catalysts for Suzuki cross-coupling. a 5 = aryl halide (0.51 mmol), boronic acid (0.61 m m ol, 1.2 eq.), potassium carbonate (212 mg, 1.53 mm o l, 3 eq.), and Pd/G (2.1 mg, 1.53 l m ol, 0.3 mol%) in 8 m L (H 20:EtOH) (1:1) were heated at 80 ° C (MWI) for 10 m in. b = …
Figure 16. Evaluation of catalysts for Heck reactions. a = Aryl bromide (0.5 1 mmol), alkene (1.02 mmol, 2 eq.), potassium carbonate (212 mg, 1.53 mm o l, 3 eq.), Pd/G (2.1 mg, 1.53 10 p mol, 0.3 mol%) in 8 mL (H 20:EtOH) (1:1) were heated at 180 " C (MWI) for 10 m in.; b = Isolated yields.
Figure 18 A and B A, Raman spectra of the original graphite sampl e, the exfoliated graphite oxide (GO) and the chemically converted graphene using MWI of GO in the presence of HH. B, Raman spectrum of the chemically converted graphene in the region of the 2D band showing a strong broad peak around …
Figure 19A and B. (a) SEM and (b) TEM images of the chemically converted graphene sheets using MWI of GO in the presence of HH.
Figure 20A-C. A F M images and cross-section analysis of the as-prepared chemically converted graphene sheets (using MWI of GO in the presence of HH) deposited from a suspension on a freshly cleaved mica substrate. No ultrasonic treatment was done on the 25 suspension. A-C show different thickness …
Figure 21. Comparison of the TGA plots of the graphite oxide and the chemically converted graphene sheets using MWI of GO in the presence of HH.
Figure 22A-C. TEM images of the chemically converted graphene sheets containing (a) Pd, (b) Cu and (c) Cu P d nanoparticles prepared by the simultaneous reduction of GO and the 30 appropriate metal salt in water using hydrazine hydrate under MWI.
Figure 23A-F. TEM images of the chemically converted graphene sheets containing Pd nanoparticles prepared by mixing separately prepared Pd nanoparticles and CCG sheets (a, b, -5-WO 2011/119961 PCT/US₂₀₁₁/029998 c), and simultaneous reduction of GO and Pd nitrate in water using hydrazine hydrate …
Figure 24A and B. (a) UV-Vis absorptions of the toluene suspensions of the graphene sheets containing Ag, A u and Cu nanoparticles prepared by the simultaneous reduction of 5 GO and the appropriate metal salt using oleylamine as a reducing agent under MW I. (b) TEM images of the graphene sheets …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
-2- The following is a complete listing of all claims in the application, with an indication of the status of each: Listing of claims: 1-5. (Cancel) canceled
A method of catalyzing chemical cross-coupling of at least two reactants of interest, comprising the steps of producing a Pd catalyst comprising nanoparticulate Pd supported on graphene by irradiating a mixture of graphite oxide (GO) and Pd metal with microwave radiation, and combining said at least two reactants of interest in th e presence of said Pd catalyst a nd under conditions which allow said Pd catalyst to catalyze said chemical cross-coupling of said at least two reactants of interest, wherein said chemical cross-couplin g is a Heck cross-couplin g reaction.
The method of claim 6, wherein said Pd catalyst is active for at least 5 coupling cycles.
The method of claim 6, wherein said Pd catalyst is substantially free of residual contaminants.
The met hod ef claim 6-A method of catalyzing chemical cross-co up ling of at least two reactants of interest, comprising the steps of producin a Pd catalyst comprising nano p articulate Pd supported on grap hene b y irradiating a mixture of graphite oxide (GO) and Pd metal with microwave radiation, and combining said at least two reactants of interest in the presence of said Pd catalyst and under conditions which allow said Pd catalyst to catal y ze said chemical cross-coupling of said at least two reactants of interest, wherein said chemical cross-coupling is selected from the group consisting of a Negish reaction, a Stille reaction, and a Buchwalk-Hartwig reaction.
The method of claim 44 6 wherein a product yield of said Heck cross-coupling reaction is at least 84%.
T he methed of elaim4 A method of catalyzing chemical cross-coupling of at least two reactants of interest, comprisin g the steps of p roducing a Pd catalyst comprising nanoparticulate Pd supported on g raphene by irradiatin g a mixture of graphite oxide (GO) and Pd metal with microwave radiation. and combining said at least two reactants of interest in the presence of said Pd catalyst and under conditions which allow said Pd catalyst to catalyze said chemical cross-coupling of said at -3- least two reactants of interest, wherein said chemical cross-coupling is a Sonogashira coupling reaction.
The method of claim 13, wherein a product yield of said Sonogashira cross-coupling reaction is at least 8 8%.
The method of claim 13, wherein said Pd catalyst is substantially free of residual contaminants.
Materials described outside the worked examples.
Pd catalyst comprising nanoparticulate Pd supported on graphene
graphite oxide
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 2. Atomic force microscopy (AFM) data of graphene sheets produced by M WI of 5 s oli d graphite oxide.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Heck cross-coupling reaction product yield | ≥ 84 % | Pd catalyst comprising nanoparticulate Pd supported on graphene |
Sonogashira cross-coupling reaction product yield |
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US 8,871,171Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 2. Atomic force microscopy (AFM) data of graphene sheets produced by M WI of 5 s oli d graphite oxide.
Figure 3A-F. X-ray diffraction (XRD) patterns of GO containing 2% metal precursors before and after the MWI of the solid. A, silver; B, cobalt; C, copper; D, iron; E, nickel; F, palladium.
Figure 4. XRD patterns of GO containing 5% metal precursors A, before and B, after the 10 MWI of the solid.
Figure 5. Photographs of solid graphite oxide containing metal salts before (top) and after (bottom) microwave irradiation (M W I) of the solid.
Figure 6A-C. TEM images of graphene sheets containing 2% (wt) Pd Nanoparticles produced by MWI of solid graphite oxide containing 2% (wt) palladium nitrate. A, 15 1 pm scale; B, 200 nm scale; C, 100 nm scale.
Figure 7A and B. (a) Small-angle XRD patterns of graphite, GO, graphene, and Pd/graphene (Pd/G) samples. (b) Small-angle XRD pattern of Pd/graphite oxide (Pd/GO) prepared by MWI of a mixture of GO and Pd nitrate solution in water without the addition of hydrazine hydrate. 20
Figure 8 A and B. (a) Raman spectra of the graphene and Pd/G samples prepared by the hydrazine hydrate (HH) MWI method in the G- and D-regions and (b) in the 2D-region.
Figure 9A and B. (a) SEM image and (b) EDS analysis of Pd/G prepared by the HH-MWI method.
Figure 10 A and B. TEM images of (a) 7.9 wt.% Pd/G and (b) 6.4 wt.% Pd/GO prepared by 25 MWI of a mixture of graphite oxide (GO) and palladium nitrate in the presence and absence of hydrazine hydrate, respectively.
Figure 11 A and B. A, Comparison of the TGA plots of graphite oxide (GO), graphene (G), and Pd/GO and Pd/G catalysts; B, Scheme of Suzuki cross-coupling reaction w ith Pd/G and Pd/GO. 30
Figure 1 2. Effect of catalyst concentrations for the Pd/G and Pd/GO on the conversion of reaction (
Figure 11 B).
Figure 13A andB. TEM images of (a) Pd/G after the 10th run and (b) Pd/GO after the 7th -4- WO 2011/119961 PCT/US₂ 01 1/029998 run.
Figure 14. XPS spectra of the Pd 3d5/2 and 3d3/2 electrons' binding energies for Pd/G and Pd/GO catalysts before and after Suzuki reactions.
Figure 15. Evaluation of catalysts for Suzuki cross-coupling. a 5 = aryl halide (0.51 mmol), boronic acid (0.61 m m ol, 1.2 eq.), potassium carbonate (212 mg, 1.53 mm o l, 3 eq.), and Pd/G (2.1 mg, 1.53 l m ol, 0.3 mol%) in 8 m L (H 20:EtOH) (1:1) were heated at 80 ° C (MWI) for 10 m in. b = …
Figure 16. Evaluation of catalysts for Heck reactions. a = Aryl bromide (0.5 1 mmol), alkene (1.02 mmol, 2 eq.), potassium carbonate (212 mg, 1.53 mm o l, 3 eq.), Pd/G (2.1 mg, 1.53 10 p mol, 0.3 mol%) in 8 mL (H 20:EtOH) (1:1) were heated at 180 " C (MWI) for 10 m in.; b = Isolated yields.
Figure 18 A and B A, Raman spectra of the original graphite sampl e, the exfoliated graphite oxide (GO) and the chemically converted graphene using MWI of GO in the presence of HH. B, Raman spectrum of the chemically converted graphene in the region of the 2D band showing a strong broad peak around …
Figure 19A and B. (a) SEM and (b) TEM images of the chemically converted graphene sheets using MWI of GO in the presence of HH.
Figure 20A-C. A F M images and cross-section analysis of the as-prepared chemically converted graphene sheets (using MWI of GO in the presence of HH) deposited from a suspension on a freshly cleaved mica substrate. No ultrasonic treatment was done on the 25 suspension. A-C show different thickness …
Figure 21. Comparison of the TGA plots of the graphite oxide and the chemically converted graphene sheets using MWI of GO in the presence of HH.
Figure 22A-C. TEM images of the chemically converted graphene sheets containing (a) Pd, (b) Cu and (c) Cu P d nanoparticles prepared by the simultaneous reduction of GO and the 30 appropriate metal salt in water using hydrazine hydrate under MWI.
Figure 23A-F. TEM images of the chemically converted graphene sheets containing Pd nanoparticles prepared by mixing separately prepared Pd nanoparticles and CCG sheets (a, b, -5-WO 2011/119961 PCT/US₂₀₁₁/029998 c), and simultaneous reduction of GO and Pd nitrate in water using hydrazine hydrate …
Figure 24A and B. (a) UV-Vis absorptions of the toluene suspensions of the graphene sheets containing Ag, A u and Cu nanoparticles prepared by the simultaneous reduction of 5 GO and the appropriate metal salt using oleylamine as a reducing agent under MW I. (b) TEM images of the graphene sheets …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
-2- The following is a complete listing of all claims in the application, with an indication of the status of each: Listing of claims: 1-5. (Cancel) canceled
A method of catalyzing chemical cross-coupling of at least two reactants of interest, comprising the steps of producing a Pd catalyst comprising nanoparticulate Pd supported on graphene by irradiating a mixture of graphite oxide (GO) and Pd metal with microwave radiation, and combining said at least two reactants of interest in th e presence of said Pd catalyst a nd under conditions which allow said Pd catalyst to catalyze said chemical cross-coupling of said at least two reactants of interest, wherein said chemical cross-couplin g is a Heck cross-couplin g reaction.
The method of claim 6, wherein said Pd catalyst is active for at least 5 coupling cycles.
The method of claim 6, wherein said Pd catalyst is substantially free of residual contaminants.
The met hod ef claim 6-A method of catalyzing chemical cross-co up ling of at least two reactants of interest, comprising the steps of producin a Pd catalyst comprising nano p articulate Pd supported on grap hene b y irradiating a mixture of graphite oxide (GO) and Pd metal with microwave radiation, and combining said at least two reactants of interest in the presence of said Pd catalyst and under conditions which allow said Pd catalyst to catal y ze said chemical cross-coupling of said at least two reactants of interest, wherein said chemical cross-coupling is selected from the group consisting of a Negish reaction, a Stille reaction, and a Buchwalk-Hartwig reaction.
The method of claim 44 6 wherein a product yield of said Heck cross-coupling reaction is at least 84%.
T he methed of elaim4 A method of catalyzing chemical cross-coupling of at least two reactants of interest, comprisin g the steps of p roducing a Pd catalyst comprising nanoparticulate Pd supported on g raphene by irradiatin g a mixture of graphite oxide (GO) and Pd metal with microwave radiation. and combining said at least two reactants of interest in the presence of said Pd catalyst and under conditions which allow said Pd catalyst to catalyze said chemical cross-coupling of said at -3- least two reactants of interest, wherein said chemical cross-coupling is a Sonogashira coupling reaction.
The method of claim 13, wherein a product yield of said Sonogashira cross-coupling reaction is at least 8 8%.
The method of claim 13, wherein said Pd catalyst is substantially free of residual contaminants.
Materials described outside the worked examples.
Pd catalyst comprising nanoparticulate Pd supported on graphene
graphite oxide
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 2. Atomic force microscopy (AFM) data of graphene sheets produced by M WI of 5 s oli d graphite oxide.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Heck cross-coupling reaction product yield | ≥ 84 % | Pd catalyst comprising nanoparticulate Pd supported on graphene |
Sonogashira cross-coupling reaction product yield |
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Patent
Atlas literature
Patent
US 8,871,171Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 2. Atomic force microscopy (AFM) data of graphene sheets produced by M WI of 5 s oli d graphite oxide.
Figure 3A-F. X-ray diffraction (XRD) patterns of GO containing 2% metal precursors before and after the MWI of the solid. A, silver; B, cobalt; C, copper; D, iron; E, nickel; F, palladium.
Figure 4. XRD patterns of GO containing 5% metal precursors A, before and B, after the 10 MWI of the solid.
Figure 5. Photographs of solid graphite oxide containing metal salts before (top) and after (bottom) microwave irradiation (M W I) of the solid.
Figure 6A-C. TEM images of graphene sheets containing 2% (wt) Pd Nanoparticles produced by MWI of solid graphite oxide containing 2% (wt) palladium nitrate. A, 15 1 pm scale; B, 200 nm scale; C, 100 nm scale.
Figure 7A and B. (a) Small-angle XRD patterns of graphite, GO, graphene, and Pd/graphene (Pd/G) samples. (b) Small-angle XRD pattern of Pd/graphite oxide (Pd/GO) prepared by MWI of a mixture of GO and Pd nitrate solution in water without the addition of hydrazine hydrate. 20
Figure 8 A and B. (a) Raman spectra of the graphene and Pd/G samples prepared by the hydrazine hydrate (HH) MWI method in the G- and D-regions and (b) in the 2D-region.
Figure 9A and B. (a) SEM image and (b) EDS analysis of Pd/G prepared by the HH-MWI method.
Figure 10 A and B. TEM images of (a) 7.9 wt.% Pd/G and (b) 6.4 wt.% Pd/GO prepared by 25 MWI of a mixture of graphite oxide (GO) and palladium nitrate in the presence and absence of hydrazine hydrate, respectively.
Figure 11 A and B. A, Comparison of the TGA plots of graphite oxide (GO), graphene (G), and Pd/GO and Pd/G catalysts; B, Scheme of Suzuki cross-coupling reaction w ith Pd/G and Pd/GO. 30
Figure 1 2. Effect of catalyst concentrations for the Pd/G and Pd/GO on the conversion of reaction (
Figure 11 B).
Figure 13A andB. TEM images of (a) Pd/G after the 10th run and (b) Pd/GO after the 7th -4- WO 2011/119961 PCT/US₂ 01 1/029998 run.
Figure 14. XPS spectra of the Pd 3d5/2 and 3d3/2 electrons' binding energies for Pd/G and Pd/GO catalysts before and after Suzuki reactions.
Figure 15. Evaluation of catalysts for Suzuki cross-coupling. a 5 = aryl halide (0.51 mmol), boronic acid (0.61 m m ol, 1.2 eq.), potassium carbonate (212 mg, 1.53 mm o l, 3 eq.), and Pd/G (2.1 mg, 1.53 l m ol, 0.3 mol%) in 8 m L (H 20:EtOH) (1:1) were heated at 80 ° C (MWI) for 10 m in. b = …
Figure 16. Evaluation of catalysts for Heck reactions. a = Aryl bromide (0.5 1 mmol), alkene (1.02 mmol, 2 eq.), potassium carbonate (212 mg, 1.53 mm o l, 3 eq.), Pd/G (2.1 mg, 1.53 10 p mol, 0.3 mol%) in 8 mL (H 20:EtOH) (1:1) were heated at 180 " C (MWI) for 10 m in.; b = Isolated yields.
Figure 18 A and B A, Raman spectra of the original graphite sampl e, the exfoliated graphite oxide (GO) and the chemically converted graphene using MWI of GO in the presence of HH. B, Raman spectrum of the chemically converted graphene in the region of the 2D band showing a strong broad peak around …
Figure 19A and B. (a) SEM and (b) TEM images of the chemically converted graphene sheets using MWI of GO in the presence of HH.
Figure 20A-C. A F M images and cross-section analysis of the as-prepared chemically converted graphene sheets (using MWI of GO in the presence of HH) deposited from a suspension on a freshly cleaved mica substrate. No ultrasonic treatment was done on the 25 suspension. A-C show different thickness …
Figure 21. Comparison of the TGA plots of the graphite oxide and the chemically converted graphene sheets using MWI of GO in the presence of HH.
Figure 22A-C. TEM images of the chemically converted graphene sheets containing (a) Pd, (b) Cu and (c) Cu P d nanoparticles prepared by the simultaneous reduction of GO and the 30 appropriate metal salt in water using hydrazine hydrate under MWI.
Figure 23A-F. TEM images of the chemically converted graphene sheets containing Pd nanoparticles prepared by mixing separately prepared Pd nanoparticles and CCG sheets (a, b, -5-WO 2011/119961 PCT/US₂₀₁₁/029998 c), and simultaneous reduction of GO and Pd nitrate in water using hydrazine hydrate …
Figure 24A and B. (a) UV-Vis absorptions of the toluene suspensions of the graphene sheets containing Ag, A u and Cu nanoparticles prepared by the simultaneous reduction of 5 GO and the appropriate metal salt using oleylamine as a reducing agent under MW I. (b) TEM images of the graphene sheets …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
-2- The following is a complete listing of all claims in the application, with an indication of the status of each: Listing of claims: 1-5. (Cancel) canceled
A method of catalyzing chemical cross-coupling of at least two reactants of interest, comprising the steps of producing a Pd catalyst comprising nanoparticulate Pd supported on graphene by irradiating a mixture of graphite oxide (GO) and Pd metal with microwave radiation, and combining said at least two reactants of interest in th e presence of said Pd catalyst a nd under conditions which allow said Pd catalyst to catalyze said chemical cross-coupling of said at least two reactants of interest, wherein said chemical cross-couplin g is a Heck cross-couplin g reaction.
The method of claim 6, wherein said Pd catalyst is active for at least 5 coupling cycles.
The method of claim 6, wherein said Pd catalyst is substantially free of residual contaminants.
The met hod ef claim 6-A method of catalyzing chemical cross-co up ling of at least two reactants of interest, comprising the steps of producin a Pd catalyst comprising nano p articulate Pd supported on grap hene b y irradiating a mixture of graphite oxide (GO) and Pd metal with microwave radiation, and combining said at least two reactants of interest in the presence of said Pd catalyst and under conditions which allow said Pd catalyst to catal y ze said chemical cross-coupling of said at least two reactants of interest, wherein said chemical cross-coupling is selected from the group consisting of a Negish reaction, a Stille reaction, and a Buchwalk-Hartwig reaction.
The method of claim 44 6 wherein a product yield of said Heck cross-coupling reaction is at least 84%.
T he methed of elaim4 A method of catalyzing chemical cross-coupling of at least two reactants of interest, comprisin g the steps of p roducing a Pd catalyst comprising nanoparticulate Pd supported on g raphene by irradiatin g a mixture of graphite oxide (GO) and Pd metal with microwave radiation. and combining said at least two reactants of interest in the presence of said Pd catalyst and under conditions which allow said Pd catalyst to catalyze said chemical cross-coupling of said at -3- least two reactants of interest, wherein said chemical cross-coupling is a Sonogashira coupling reaction.
The method of claim 13, wherein a product yield of said Sonogashira cross-coupling reaction is at least 8 8%.
The method of claim 13, wherein said Pd catalyst is substantially free of residual contaminants.
Materials described outside the worked examples.
Pd catalyst comprising nanoparticulate Pd supported on graphene
graphite oxide
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 2. Atomic force microscopy (AFM) data of graphene sheets produced by M WI of 5 s oli d graphite oxide.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Heck cross-coupling reaction product yield | ≥ 84 % | Pd catalyst comprising nanoparticulate Pd supported on graphene |
Sonogashira cross-coupling reaction product yield |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
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US 8,871,171Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 2. Atomic force microscopy (AFM) data of graphene sheets produced by M WI of 5 s oli d graphite oxide.
Figure 3A-F. X-ray diffraction (XRD) patterns of GO containing 2% metal precursors before and after the MWI of the solid. A, silver; B, cobalt; C, copper; D, iron; E, nickel; F, palladium.
Figure 4. XRD patterns of GO containing 5% metal precursors A, before and B, after the 10 MWI of the solid.
Figure 5. Photographs of solid graphite oxide containing metal salts before (top) and after (bottom) microwave irradiation (M W I) of the solid.
Figure 6A-C. TEM images of graphene sheets containing 2% (wt) Pd Nanoparticles produced by MWI of solid graphite oxide containing 2% (wt) palladium nitrate. A, 15 1 pm scale; B, 200 nm scale; C, 100 nm scale.
Figure 7A and B. (a) Small-angle XRD patterns of graphite, GO, graphene, and Pd/graphene (Pd/G) samples. (b) Small-angle XRD pattern of Pd/graphite oxide (Pd/GO) prepared by MWI of a mixture of GO and Pd nitrate solution in water without the addition of hydrazine hydrate. 20
Figure 8 A and B. (a) Raman spectra of the graphene and Pd/G samples prepared by the hydrazine hydrate (HH) MWI method in the G- and D-regions and (b) in the 2D-region.
Figure 9A and B. (a) SEM image and (b) EDS analysis of Pd/G prepared by the HH-MWI method.
Figure 10 A and B. TEM images of (a) 7.9 wt.% Pd/G and (b) 6.4 wt.% Pd/GO prepared by 25 MWI of a mixture of graphite oxide (GO) and palladium nitrate in the presence and absence of hydrazine hydrate, respectively.
Figure 11 A and B. A, Comparison of the TGA plots of graphite oxide (GO), graphene (G), and Pd/GO and Pd/G catalysts; B, Scheme of Suzuki cross-coupling reaction w ith Pd/G and Pd/GO. 30
Figure 1 2. Effect of catalyst concentrations for the Pd/G and Pd/GO on the conversion of reaction (
Figure 11 B).
Figure 13A andB. TEM images of (a) Pd/G after the 10th run and (b) Pd/GO after the 7th -4- WO 2011/119961 PCT/US₂ 01 1/029998 run.
Figure 14. XPS spectra of the Pd 3d5/2 and 3d3/2 electrons' binding energies for Pd/G and Pd/GO catalysts before and after Suzuki reactions.
Figure 15. Evaluation of catalysts for Suzuki cross-coupling. a 5 = aryl halide (0.51 mmol), boronic acid (0.61 m m ol, 1.2 eq.), potassium carbonate (212 mg, 1.53 mm o l, 3 eq.), and Pd/G (2.1 mg, 1.53 l m ol, 0.3 mol%) in 8 m L (H 20:EtOH) (1:1) were heated at 80 ° C (MWI) for 10 m in. b = …
Figure 16. Evaluation of catalysts for Heck reactions. a = Aryl bromide (0.5 1 mmol), alkene (1.02 mmol, 2 eq.), potassium carbonate (212 mg, 1.53 mm o l, 3 eq.), Pd/G (2.1 mg, 1.53 10 p mol, 0.3 mol%) in 8 mL (H 20:EtOH) (1:1) were heated at 180 " C (MWI) for 10 m in.; b = Isolated yields.
Figure 18 A and B A, Raman spectra of the original graphite sampl e, the exfoliated graphite oxide (GO) and the chemically converted graphene using MWI of GO in the presence of HH. B, Raman spectrum of the chemically converted graphene in the region of the 2D band showing a strong broad peak around …
Figure 19A and B. (a) SEM and (b) TEM images of the chemically converted graphene sheets using MWI of GO in the presence of HH.
Figure 20A-C. A F M images and cross-section analysis of the as-prepared chemically converted graphene sheets (using MWI of GO in the presence of HH) deposited from a suspension on a freshly cleaved mica substrate. No ultrasonic treatment was done on the 25 suspension. A-C show different thickness …
Figure 21. Comparison of the TGA plots of the graphite oxide and the chemically converted graphene sheets using MWI of GO in the presence of HH.
Figure 22A-C. TEM images of the chemically converted graphene sheets containing (a) Pd, (b) Cu and (c) Cu P d nanoparticles prepared by the simultaneous reduction of GO and the 30 appropriate metal salt in water using hydrazine hydrate under MWI.
Figure 23A-F. TEM images of the chemically converted graphene sheets containing Pd nanoparticles prepared by mixing separately prepared Pd nanoparticles and CCG sheets (a, b, -5-WO 2011/119961 PCT/US₂₀₁₁/029998 c), and simultaneous reduction of GO and Pd nitrate in water using hydrazine hydrate …
Figure 24A and B. (a) UV-Vis absorptions of the toluene suspensions of the graphene sheets containing Ag, A u and Cu nanoparticles prepared by the simultaneous reduction of 5 GO and the appropriate metal salt using oleylamine as a reducing agent under MW I. (b) TEM images of the graphene sheets …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
-2- The following is a complete listing of all claims in the application, with an indication of the status of each: Listing of claims: 1-5. (Cancel) canceled
A method of catalyzing chemical cross-coupling of at least two reactants of interest, comprising the steps of producing a Pd catalyst comprising nanoparticulate Pd supported on graphene by irradiating a mixture of graphite oxide (GO) and Pd metal with microwave radiation, and combining said at least two reactants of interest in th e presence of said Pd catalyst a nd under conditions which allow said Pd catalyst to catalyze said chemical cross-coupling of said at least two reactants of interest, wherein said chemical cross-couplin g is a Heck cross-couplin g reaction.
The method of claim 6, wherein said Pd catalyst is active for at least 5 coupling cycles.
The method of claim 6, wherein said Pd catalyst is substantially free of residual contaminants.
The met hod ef claim 6-A method of catalyzing chemical cross-co up ling of at least two reactants of interest, comprising the steps of producin a Pd catalyst comprising nano p articulate Pd supported on grap hene b y irradiating a mixture of graphite oxide (GO) and Pd metal with microwave radiation, and combining said at least two reactants of interest in the presence of said Pd catalyst and under conditions which allow said Pd catalyst to catal y ze said chemical cross-coupling of said at least two reactants of interest, wherein said chemical cross-coupling is selected from the group consisting of a Negish reaction, a Stille reaction, and a Buchwalk-Hartwig reaction.
The method of claim 44 6 wherein a product yield of said Heck cross-coupling reaction is at least 84%.
T he methed of elaim4 A method of catalyzing chemical cross-coupling of at least two reactants of interest, comprisin g the steps of p roducing a Pd catalyst comprising nanoparticulate Pd supported on g raphene by irradiatin g a mixture of graphite oxide (GO) and Pd metal with microwave radiation. and combining said at least two reactants of interest in the presence of said Pd catalyst and under conditions which allow said Pd catalyst to catalyze said chemical cross-coupling of said at -3- least two reactants of interest, wherein said chemical cross-coupling is a Sonogashira coupling reaction.
The method of claim 13, wherein a product yield of said Sonogashira cross-coupling reaction is at least 8 8%.
The method of claim 13, wherein said Pd catalyst is substantially free of residual contaminants.
Materials described outside the worked examples.
Pd catalyst comprising nanoparticulate Pd supported on graphene
graphite oxide
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 2. Atomic force microscopy (AFM) data of graphene sheets produced by M WI of 5 s oli d graphite oxide.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Heck cross-coupling reaction product yield | ≥ 84 % | Pd catalyst comprising nanoparticulate Pd supported on graphene |
Sonogashira cross-coupling reaction product yield |
Related documents with shared materials, methods, properties, or citations.
Pd metal
Pd
graphene
Pd salt (Pd nitrate, Pd acetate)
Figure 3A-F. X-ray diffraction (XRD) patterns of GO containing 2% metal precursors before and after the MWI of the solid. A, silver; B, cobalt; C, copper; D, iron; E, nickel; F, palladium.
Figure 4. XRD patterns of GO containing 5% metal precursors A, before and B, after the 10 MWI of the solid.
Figure 6A-C. TEM images of graphene sheets containing 2% (wt) Pd Nanoparticles produced by MWI of solid graphite oxide containing 2% (wt) palladium nitrate. A, 15 1 pm scale; B, 200 nm scale; C, 100 nm scale.
Figure 7A and B. (a) Small-angle XRD patterns of graphite, GO, graphene, and Pd/graphene (Pd/G) samples. (b) Small-angle XRD pattern of Pd/graphite oxide (Pd/GO) prepared by MWI of a mixture of GO and Pd nitrate solution in water without the addition of hydrazine hydrate. 20
Figure 8 A and B. (a) Raman spectra of the graphene and Pd/G samples prepared by the hydrazine hydrate (HH) MWI method in the G- and D-regions and (b) in the 2D-region.
Figure 9A and B. (a) SEM image and (b) EDS analysis of Pd/G prepared by the HH-MWI method.
Figure 10 A and B. TEM images of (a) 7.9 wt.% Pd/G and (b) 6.4 wt.% Pd/GO prepared by 25 MWI of a mixture of graphite oxide (GO) and palladium nitrate in the presence and absence of hydrazine hydrate, respectively.
Figure 13A andB. TEM images of (a) Pd/G after the 10th run and (b) Pd/GO after the 7th -4- WO 2011/119961 PCT/US₂ 01 1/029998 run.
Figure 14. XPS spectra of the Pd 3d5/2 and 3d3/2 electrons' binding energies for Pd/G and Pd/GO catalysts before and after Suzuki reactions.
Figure 18 A and B A, Raman spectra of the original graphite sampl e, the exfoliated graphite oxide (GO) and the chemically converted graphene using MWI of GO in the presence of HH. B, Raman spectrum of the chemically converted graphene in the region of the 2D band showing a strong broad peak around …
Figure 19A and B. (a) SEM and (b) TEM images of the chemically converted graphene sheets using MWI of GO in the presence of HH.
Figure 19A and B. (a) SEM and (b) TEM images of the chemically converted graphene sheets using MWI of GO in the presence of HH.
Figure 20A-C. A F M images and cross-section analysis of the as-prepared chemically converted graphene sheets (using MWI of GO in the presence of HH) deposited from a suspension on a freshly cleaved mica substrate. No ultrasonic treatment was done on the 25 suspension. A-C show different thickness …
Figure 22A-C. TEM images of the chemically converted graphene sheets containing (a) Pd, (b) Cu and (c) Cu P d nanoparticles prepared by the simultaneous reduction of GO and the 30 appropriate metal salt in water using hydrazine hydrate under MWI.
Figure 23A-F. TEM images of the chemically converted graphene sheets containing Pd nanoparticles prepared by mixing separately prepared Pd nanoparticles and CCG sheets (a, b, -5-WO 2011/119961 PCT/US₂₀₁₁/029998 c), and simultaneous reduction of GO and Pd nitrate in water using hydrazine hydrate …
Figure 24A and B. (a) UV-Vis absorptions of the toluene suspensions of the graphene sheets containing Ag, A u and Cu nanoparticles prepared by the simultaneous reduction of 5 GO and the appropriate metal salt using oleylamine as a reducing agent under MW I. (b) TEM images of the graphene sheets …
Figure 24A and B. (a) UV-Vis absorptions of the toluene suspensions of the graphene sheets containing Ag, A u and Cu nanoparticles prepared by the simultaneous reduction of 5 GO and the appropriate metal salt using oleylamine as a reducing agent under MW I. (b) TEM images of the graphene sheets …
ot shown). At lower catalyst loading of 0.1 mo l %, Pd/G yields the product with 100% conversion after 2.5 h, in comparison with 20 95% with
| ≥ 88 % |
Pd catalyst comprising nanoparticulate Pd supported on graphene |
Suzuki cross-coupling reaction product yield | ≥ 65 % | Pd catalyst comprising nanoparticulate Pd supported on graphene |
Pd catalyst turnover frequency for Suzuki cross-coupling | ≥ 100000 h^-1 | Pd catalyst comprising nanoparticulate Pd supported on graphene |
Pd catalyst active coupling cycles | ≥ 5 cycles | Pd catalyst comprising nanoparticulate Pd supported on graphene |
Duration | 10–300 s | — |
Thickness | 7–9 nm | — |
Thickness | 12–15 nm | — |
Thickness | 4–6 nm | — |
Temperature | ≤ 1 °C | — |
Thickness | ≥ 2700 cm | — |
Duration | 10–600 s | — |
Thickness | 10–5000 nm | — |
Thickness | 50–2500 nm | — |
Thickness | 100–1000 nm | — |
Thickness | 1–20 nm | — |
Thickness | 1–10 cm | — |
Duration | 1–10 minutes | — |
Temperature | 20–25 °C | — |
Temperature | 1–2 °C | — |
Temperature | ≤ 0 °C | — |
Pd metal
Pd
graphene
Pd salt (Pd nitrate, Pd acetate)
Figure 3A-F. X-ray diffraction (XRD) patterns of GO containing 2% metal precursors before and after the MWI of the solid. A, silver; B, cobalt; C, copper; D, iron; E, nickel; F, palladium.
Figure 4. XRD patterns of GO containing 5% metal precursors A, before and B, after the 10 MWI of the solid.
Figure 6A-C. TEM images of graphene sheets containing 2% (wt) Pd Nanoparticles produced by MWI of solid graphite oxide containing 2% (wt) palladium nitrate. A, 15 1 pm scale; B, 200 nm scale; C, 100 nm scale.
Figure 7A and B. (a) Small-angle XRD patterns of graphite, GO, graphene, and Pd/graphene (Pd/G) samples. (b) Small-angle XRD pattern of Pd/graphite oxide (Pd/GO) prepared by MWI of a mixture of GO and Pd nitrate solution in water without the addition of hydrazine hydrate. 20
Figure 8 A and B. (a) Raman spectra of the graphene and Pd/G samples prepared by the hydrazine hydrate (HH) MWI method in the G- and D-regions and (b) in the 2D-region.
Figure 9A and B. (a) SEM image and (b) EDS analysis of Pd/G prepared by the HH-MWI method.
Figure 10 A and B. TEM images of (a) 7.9 wt.% Pd/G and (b) 6.4 wt.% Pd/GO prepared by 25 MWI of a mixture of graphite oxide (GO) and palladium nitrate in the presence and absence of hydrazine hydrate, respectively.
Figure 13A andB. TEM images of (a) Pd/G after the 10th run and (b) Pd/GO after the 7th -4- WO 2011/119961 PCT/US₂ 01 1/029998 run.
Figure 14. XPS spectra of the Pd 3d5/2 and 3d3/2 electrons' binding energies for Pd/G and Pd/GO catalysts before and after Suzuki reactions.
Figure 18 A and B A, Raman spectra of the original graphite sampl e, the exfoliated graphite oxide (GO) and the chemically converted graphene using MWI of GO in the presence of HH. B, Raman spectrum of the chemically converted graphene in the region of the 2D band showing a strong broad peak around …
Figure 19A and B. (a) SEM and (b) TEM images of the chemically converted graphene sheets using MWI of GO in the presence of HH.
Figure 19A and B. (a) SEM and (b) TEM images of the chemically converted graphene sheets using MWI of GO in the presence of HH.
Figure 20A-C. A F M images and cross-section analysis of the as-prepared chemically converted graphene sheets (using MWI of GO in the presence of HH) deposited from a suspension on a freshly cleaved mica substrate. No ultrasonic treatment was done on the 25 suspension. A-C show different thickness …
Figure 22A-C. TEM images of the chemically converted graphene sheets containing (a) Pd, (b) Cu and (c) Cu P d nanoparticles prepared by the simultaneous reduction of GO and the 30 appropriate metal salt in water using hydrazine hydrate under MWI.
Figure 23A-F. TEM images of the chemically converted graphene sheets containing Pd nanoparticles prepared by mixing separately prepared Pd nanoparticles and CCG sheets (a, b, -5-WO 2011/119961 PCT/US₂₀₁₁/029998 c), and simultaneous reduction of GO and Pd nitrate in water using hydrazine hydrate …
Figure 24A and B. (a) UV-Vis absorptions of the toluene suspensions of the graphene sheets containing Ag, A u and Cu nanoparticles prepared by the simultaneous reduction of 5 GO and the appropriate metal salt using oleylamine as a reducing agent under MW I. (b) TEM images of the graphene sheets …
Figure 24A and B. (a) UV-Vis absorptions of the toluene suspensions of the graphene sheets containing Ag, A u and Cu nanoparticles prepared by the simultaneous reduction of 5 GO and the appropriate metal salt using oleylamine as a reducing agent under MW I. (b) TEM images of the graphene sheets …
ot shown). At lower catalyst loading of 0.1 mo l %, Pd/G yields the product with 100% conversion after 2.5 h, in comparison with 20 95% with
| ≥ 88 % |
Pd catalyst comprising nanoparticulate Pd supported on graphene |
Suzuki cross-coupling reaction product yield | ≥ 65 % | Pd catalyst comprising nanoparticulate Pd supported on graphene |
Pd catalyst turnover frequency for Suzuki cross-coupling | ≥ 100000 h^-1 | Pd catalyst comprising nanoparticulate Pd supported on graphene |
Pd catalyst active coupling cycles | ≥ 5 cycles | Pd catalyst comprising nanoparticulate Pd supported on graphene |
Duration | 10–300 s | — |
Thickness | 7–9 nm | — |
Thickness | 12–15 nm | — |
Thickness | 4–6 nm | — |
Temperature | ≤ 1 °C | — |
Thickness | ≥ 2700 cm | — |
Duration | 10–600 s | — |
Thickness | 10–5000 nm | — |
Thickness | 50–2500 nm | — |
Thickness | 100–1000 nm | — |
Thickness | 1–20 nm | — |
Thickness | 1–10 cm | — |
Duration | 1–10 minutes | — |
Temperature | 20–25 °C | — |
Temperature | 1–2 °C | — |
Temperature | ≤ 0 °C | — |
Pd metal
Pd
graphene
Pd salt (Pd nitrate, Pd acetate)
Figure 3A-F. X-ray diffraction (XRD) patterns of GO containing 2% metal precursors before and after the MWI of the solid. A, silver; B, cobalt; C, copper; D, iron; E, nickel; F, palladium.
Figure 4. XRD patterns of GO containing 5% metal precursors A, before and B, after the 10 MWI of the solid.
Figure 6A-C. TEM images of graphene sheets containing 2% (wt) Pd Nanoparticles produced by MWI of solid graphite oxide containing 2% (wt) palladium nitrate. A, 15 1 pm scale; B, 200 nm scale; C, 100 nm scale.
Figure 7A and B. (a) Small-angle XRD patterns of graphite, GO, graphene, and Pd/graphene (Pd/G) samples. (b) Small-angle XRD pattern of Pd/graphite oxide (Pd/GO) prepared by MWI of a mixture of GO and Pd nitrate solution in water without the addition of hydrazine hydrate. 20
Figure 8 A and B. (a) Raman spectra of the graphene and Pd/G samples prepared by the hydrazine hydrate (HH) MWI method in the G- and D-regions and (b) in the 2D-region.
Figure 9A and B. (a) SEM image and (b) EDS analysis of Pd/G prepared by the HH-MWI method.
Figure 10 A and B. TEM images of (a) 7.9 wt.% Pd/G and (b) 6.4 wt.% Pd/GO prepared by 25 MWI of a mixture of graphite oxide (GO) and palladium nitrate in the presence and absence of hydrazine hydrate, respectively.
Figure 13A andB. TEM images of (a) Pd/G after the 10th run and (b) Pd/GO after the 7th -4- WO 2011/119961 PCT/US₂ 01 1/029998 run.
Figure 14. XPS spectra of the Pd 3d5/2 and 3d3/2 electrons' binding energies for Pd/G and Pd/GO catalysts before and after Suzuki reactions.
Figure 18 A and B A, Raman spectra of the original graphite sampl e, the exfoliated graphite oxide (GO) and the chemically converted graphene using MWI of GO in the presence of HH. B, Raman spectrum of the chemically converted graphene in the region of the 2D band showing a strong broad peak around …
Figure 19A and B. (a) SEM and (b) TEM images of the chemically converted graphene sheets using MWI of GO in the presence of HH.
Figure 19A and B. (a) SEM and (b) TEM images of the chemically converted graphene sheets using MWI of GO in the presence of HH.
Figure 20A-C. A F M images and cross-section analysis of the as-prepared chemically converted graphene sheets (using MWI of GO in the presence of HH) deposited from a suspension on a freshly cleaved mica substrate. No ultrasonic treatment was done on the 25 suspension. A-C show different thickness …
Figure 22A-C. TEM images of the chemically converted graphene sheets containing (a) Pd, (b) Cu and (c) Cu P d nanoparticles prepared by the simultaneous reduction of GO and the 30 appropriate metal salt in water using hydrazine hydrate under MWI.
Figure 23A-F. TEM images of the chemically converted graphene sheets containing Pd nanoparticles prepared by mixing separately prepared Pd nanoparticles and CCG sheets (a, b, -5-WO 2011/119961 PCT/US₂₀₁₁/029998 c), and simultaneous reduction of GO and Pd nitrate in water using hydrazine hydrate …
Figure 24A and B. (a) UV-Vis absorptions of the toluene suspensions of the graphene sheets containing Ag, A u and Cu nanoparticles prepared by the simultaneous reduction of 5 GO and the appropriate metal salt using oleylamine as a reducing agent under MW I. (b) TEM images of the graphene sheets …
Figure 24A and B. (a) UV-Vis absorptions of the toluene suspensions of the graphene sheets containing Ag, A u and Cu nanoparticles prepared by the simultaneous reduction of 5 GO and the appropriate metal salt using oleylamine as a reducing agent under MW I. (b) TEM images of the graphene sheets …
ot shown). At lower catalyst loading of 0.1 mo l %, Pd/G yields the product with 100% conversion after 2.5 h, in comparison with 20 95% with
| ≥ 88 % |
Pd catalyst comprising nanoparticulate Pd supported on graphene |
Suzuki cross-coupling reaction product yield | ≥ 65 % | Pd catalyst comprising nanoparticulate Pd supported on graphene |
Pd catalyst turnover frequency for Suzuki cross-coupling | ≥ 100000 h^-1 | Pd catalyst comprising nanoparticulate Pd supported on graphene |
Pd catalyst active coupling cycles | ≥ 5 cycles | Pd catalyst comprising nanoparticulate Pd supported on graphene |
Duration | 10–300 s | — |
Thickness | 7–9 nm | — |
Thickness | 12–15 nm | — |
Thickness | 4–6 nm | — |
Temperature | ≤ 1 °C | — |
Thickness | ≥ 2700 cm | — |
Duration | 10–600 s | — |
Thickness | 10–5000 nm | — |
Thickness | 50–2500 nm | — |
Thickness | 100–1000 nm | — |
Thickness | 1–20 nm | — |
Thickness | 1–10 cm | — |
Duration | 1–10 minutes | — |
Temperature | 20–25 °C | — |
Temperature | 1–2 °C | — |
Temperature | ≤ 0 °C | — |
Pd metal
Pd
graphene
Pd salt (Pd nitrate, Pd acetate)
Figure 3A-F. X-ray diffraction (XRD) patterns of GO containing 2% metal precursors before and after the MWI of the solid. A, silver; B, cobalt; C, copper; D, iron; E, nickel; F, palladium.
Figure 4. XRD patterns of GO containing 5% metal precursors A, before and B, after the 10 MWI of the solid.
Figure 6A-C. TEM images of graphene sheets containing 2% (wt) Pd Nanoparticles produced by MWI of solid graphite oxide containing 2% (wt) palladium nitrate. A, 15 1 pm scale; B, 200 nm scale; C, 100 nm scale.
Figure 7A and B. (a) Small-angle XRD patterns of graphite, GO, graphene, and Pd/graphene (Pd/G) samples. (b) Small-angle XRD pattern of Pd/graphite oxide (Pd/GO) prepared by MWI of a mixture of GO and Pd nitrate solution in water without the addition of hydrazine hydrate. 20
Figure 8 A and B. (a) Raman spectra of the graphene and Pd/G samples prepared by the hydrazine hydrate (HH) MWI method in the G- and D-regions and (b) in the 2D-region.
Figure 9A and B. (a) SEM image and (b) EDS analysis of Pd/G prepared by the HH-MWI method.
Figure 10 A and B. TEM images of (a) 7.9 wt.% Pd/G and (b) 6.4 wt.% Pd/GO prepared by 25 MWI of a mixture of graphite oxide (GO) and palladium nitrate in the presence and absence of hydrazine hydrate, respectively.
Figure 13A andB. TEM images of (a) Pd/G after the 10th run and (b) Pd/GO after the 7th -4- WO 2011/119961 PCT/US₂ 01 1/029998 run.
Figure 14. XPS spectra of the Pd 3d5/2 and 3d3/2 electrons' binding energies for Pd/G and Pd/GO catalysts before and after Suzuki reactions.
Figure 18 A and B A, Raman spectra of the original graphite sampl e, the exfoliated graphite oxide (GO) and the chemically converted graphene using MWI of GO in the presence of HH. B, Raman spectrum of the chemically converted graphene in the region of the 2D band showing a strong broad peak around …
Figure 19A and B. (a) SEM and (b) TEM images of the chemically converted graphene sheets using MWI of GO in the presence of HH.
Figure 19A and B. (a) SEM and (b) TEM images of the chemically converted graphene sheets using MWI of GO in the presence of HH.
Figure 20A-C. A F M images and cross-section analysis of the as-prepared chemically converted graphene sheets (using MWI of GO in the presence of HH) deposited from a suspension on a freshly cleaved mica substrate. No ultrasonic treatment was done on the 25 suspension. A-C show different thickness …
Figure 22A-C. TEM images of the chemically converted graphene sheets containing (a) Pd, (b) Cu and (c) Cu P d nanoparticles prepared by the simultaneous reduction of GO and the 30 appropriate metal salt in water using hydrazine hydrate under MWI.
Figure 23A-F. TEM images of the chemically converted graphene sheets containing Pd nanoparticles prepared by mixing separately prepared Pd nanoparticles and CCG sheets (a, b, -5-WO 2011/119961 PCT/US₂₀₁₁/029998 c), and simultaneous reduction of GO and Pd nitrate in water using hydrazine hydrate …
Figure 24A and B. (a) UV-Vis absorptions of the toluene suspensions of the graphene sheets containing Ag, A u and Cu nanoparticles prepared by the simultaneous reduction of 5 GO and the appropriate metal salt using oleylamine as a reducing agent under MW I. (b) TEM images of the graphene sheets …
Figure 24A and B. (a) UV-Vis absorptions of the toluene suspensions of the graphene sheets containing Ag, A u and Cu nanoparticles prepared by the simultaneous reduction of 5 GO and the appropriate metal salt using oleylamine as a reducing agent under MW I. (b) TEM images of the graphene sheets …
ot shown). At lower catalyst loading of 0.1 mo l %, Pd/G yields the product with 100% conversion after 2.5 h, in comparison with 20 95% with
| ≥ 88 % |
Pd catalyst comprising nanoparticulate Pd supported on graphene |
Suzuki cross-coupling reaction product yield | ≥ 65 % | Pd catalyst comprising nanoparticulate Pd supported on graphene |
Pd catalyst turnover frequency for Suzuki cross-coupling | ≥ 100000 h^-1 | Pd catalyst comprising nanoparticulate Pd supported on graphene |
Pd catalyst active coupling cycles | ≥ 5 cycles | Pd catalyst comprising nanoparticulate Pd supported on graphene |
Duration | 10–300 s | — |
Thickness | 7–9 nm | — |
Thickness | 12–15 nm | — |
Thickness | 4–6 nm | — |
Temperature | ≤ 1 °C | — |
Thickness | ≥ 2700 cm | — |
Duration | 10–600 s | — |
Thickness | 10–5000 nm | — |
Thickness | 50–2500 nm | — |
Thickness | 100–1000 nm | — |
Thickness | 1–20 nm | — |
Thickness | 1–10 cm | — |
Duration | 1–10 minutes | — |
Temperature | 20–25 °C | — |
Temperature | 1–2 °C | — |
Temperature | ≤ 0 °C | — |
