INQUIMAE   12526
INSTITUTO DE QUIMICA, FISICA DE LOS MATERIALES, MEDIOAMBIENTE Y ENERGIA
Unidad Ejecutora - UE
congresos y reuniones científicas
Título:
Palladium Nanocatalyst Electrodeposited from
Autor/es:
MIGUEL VAGO; MARIO TAGLIAZUCCHI; FEDERICO WILLIAMS; ERNESTO JULIO CALVO
Lugar:
Sevilla, España
Reunión:
Congreso; 59th Annual Meeting of the International Society of Electrochemistry; 2008
Institución organizadora:
International Society of Electrochemistry
Resumen:
We report a new method to form Pd nanoparticles by electrochemical reduction of
PdCl4
2- on carbon electrodes (glassy carbon and carbon felts supports). We employ a
self-assembled polyelectrolyte multilayer (PEM) nanoreactor1 comprised of poly(allylamine)
and poly(acrylic) acid, with further uptake of palladium ions from aqueous
solution and electrochemical reduction under potentiostatic control. The as-prepared
electrodes have been characterized by XPS, SEM and cyclic voltammetry and the
palladium content was determined by ICP elemental analysis. Furthermore, the nanoelectrocatalyst
has been assessed by studying the electrochemical hydrogenation of
acetophenone2 as a model compound.
Both, SEM images (see figure) and XPS show that the electrochemically generated Pd
nanoparticles are preferentially located at the electrode/film interface, in contrast with
the homogeneous distribution observed when a chemical reduction route is used1.
Cyclic voltammetry shows the typical response of a polycrystalline Pd electrode3. The
anodic hydrogen peak is completely suppressed in the presence of acetophenone which
confirms the electrocatalytic activity. These properties were tested in batch process and
followed by HPLC. Complete reduction of acetophenone to ethyl benzene with a
current efficiency of 84% has been observed. In addition, the electrocatalytic
performance was compared with that of an electrode bearing Pd microcrystals prepared
by direct electroreduction of Pd(II) salts2,3 on the carbon surface resulting in a
reduction rate per mole of Pd ten-fold faster than for the microcrystalline Pd electrode
prepared by the standard method
(1) Joly, S.; Kane, R.; Radzilowski, L.; Wang, T.; Wu, A.; Cohen, R. E.; Thomas, E.
L.; Rubner, M. F. Langmuir 2000, 16, 1354.
(2) Polcaro, A.; Palmas, S.; Dernini, S. Ind. Eng. Chem. Res. 1993, 32, 1315.
(3) Pattabiraman, R., Applied Catalysis A. 1997, 153, 9.4
2- on carbon electrodes (glassy carbon and carbon felts supports). We employ a
self-assembled polyelectrolyte multilayer (PEM) nanoreactor1 comprised of poly(allylamine)
and poly(acrylic) acid, with further uptake of palladium ions from aqueous
solution and electrochemical reduction under potentiostatic control. The as-prepared
electrodes have been characterized by XPS, SEM and cyclic voltammetry and the
palladium content was determined by ICP elemental analysis. Furthermore, the nanoelectrocatalyst
has been assessed by studying the electrochemical hydrogenation of
acetophenone2 as a model compound.
Both, SEM images (see figure) and XPS show that the electrochemically generated Pd
nanoparticles are preferentially located at the electrode/film interface, in contrast with
the homogeneous distribution observed when a chemical reduction route is used1.
Cyclic voltammetry shows the typical response of a polycrystalline Pd electrode3. The
anodic hydrogen peak is completely suppressed in the presence of acetophenone which
confirms the electrocatalytic activity. These properties were tested in batch process and
followed by HPLC. Complete reduction of acetophenone to ethyl benzene with a
current efficiency of 84% has been observed. In addition, the electrocatalytic
performance was compared with that of an electrode bearing Pd microcrystals prepared
by direct electroreduction of Pd(II) salts2,3 on the carbon surface resulting in a
reduction rate per mole of Pd ten-fold faster than for the microcrystalline Pd electrode
prepared by the standard method
(1) Joly, S.; Kane, R.; Radzilowski, L.; Wang, T.; Wu, A.; Cohen, R. E.; Thomas, E.
L.; Rubner, M. F. Langmuir 2000, 16, 1354.
(2) Polcaro, A.; Palmas, S.; Dernini, S. Ind. Eng. Chem. Res. 1993, 32, 1315.
(3) Pattabiraman, R., Applied Catalysis A. 1997, 153, 9.on carbon electrodes (glassy carbon and carbon felts supports). We employ a
self-assembled polyelectrolyte multilayer (PEM) nanoreactor1 comprised of poly(allylamine)
and poly(acrylic) acid, with further uptake of palladium ions from aqueous
solution and electrochemical reduction under potentiostatic control. The as-prepared
electrodes have been characterized by XPS, SEM and cyclic voltammetry and the
palladium content was determined by ICP elemental analysis. Furthermore, the nanoelectrocatalyst
has been assessed by studying the electrochemical hydrogenation of
acetophenone2 as a model compound.
Both, SEM images (see figure) and XPS show that the electrochemically generated Pd
nanoparticles are preferentially located at the electrode/film interface, in contrast with
the homogeneous distribution observed when a chemical reduction route is used1.
Cyclic voltammetry shows the typical response of a polycrystalline Pd electrode3. The
anodic hydrogen peak is completely suppressed in the presence of acetophenone which
confirms the electrocatalytic activity. These properties were tested in batch process and
followed by HPLC. Complete reduction of acetophenone to ethyl benzene with a
current efficiency of 84% has been observed. In addition, the electrocatalytic
performance was compared with that of an electrode bearing Pd microcrystals prepared
by direct electroreduction of Pd(II) salts2,3 on the carbon surface resulting in a
reduction rate per mole of Pd ten-fold faster than for the microcrystalline Pd electrode
prepared by the standard method
(1) Joly, S.; Kane, R.; Radzilowski, L.; Wang, T.; Wu, A.; Cohen, R. E.; Thomas, E.
L.; Rubner, M. F. Langmuir 2000, 16, 1354.
(2) Polcaro, A.; Palmas, S.; Dernini, S. Ind. Eng. Chem. Res. 1993, 32, 1315.
(3) Pattabiraman, R., Applied Catalysis A. 1997, 153, 9.1 comprised of poly(allylamine)
and poly(acrylic) acid, with further uptake of palladium ions from aqueous
solution and electrochemical reduction under potentiostatic control. The as-prepared
electrodes have been characterized by XPS, SEM and cyclic voltammetry and the
palladium content was determined by ICP elemental analysis. Furthermore, the nanoelectrocatalyst
has been assessed by studying the electrochemical hydrogenation of
acetophenone2 as a model compound.
Both, SEM images (see figure) and XPS show that the electrochemically generated Pd
nanoparticles are preferentially located at the electrode/film interface, in contrast with
the homogeneous distribution observed when a chemical reduction route is used1.
Cyclic voltammetry shows the typical response of a polycrystalline Pd electrode3. The
anodic hydrogen peak is completely suppressed in the presence of acetophenone which
confirms the electrocatalytic activity. These properties were tested in batch process and
followed by HPLC. Complete reduction of acetophenone to ethyl benzene with a
current efficiency of 84% has been observed. In addition, the electrocatalytic
performance was compared with that of an electrode bearing Pd microcrystals prepared
by direct electroreduction of Pd(II) salts2,3 on the carbon surface resulting in a
reduction rate per mole of Pd ten-fold faster than for the microcrystalline Pd electrode
prepared by the standard method
(1) Joly, S.; Kane, R.; Radzilowski, L.; Wang, T.; Wu, A.; Cohen, R. E.; Thomas, E.
L.; Rubner, M. F. Langmuir 2000, 16, 1354.
(2) Polcaro, A.; Palmas, S.; Dernini, S. Ind. Eng. Chem. Res. 1993, 32, 1315.
(3) Pattabiraman, R., Applied Catalysis A. 1997, 153, 9.2 as a model compound.
Both, SEM images (see figure) and XPS show that the electrochemically generated Pd
nanoparticles are preferentially located at the electrode/film interface, in contrast with
the homogeneous distribution observed when a chemical reduction route is used1.
Cyclic voltammetry shows the typical response of a polycrystalline Pd electrode3. The
anodic hydrogen peak is completely suppressed in the presence of acetophenone which
confirms the electrocatalytic activity. These properties were tested in batch process and
followed by HPLC. Complete reduction of acetophenone to ethyl benzene with a
current efficiency of 84% has been observed. In addition, the electrocatalytic
performance was compared with that of an electrode bearing Pd microcrystals prepared
by direct electroreduction of Pd(II) salts2,3 on the carbon surface resulting in a
reduction rate per mole of Pd ten-fold faster than for the microcrystalline Pd electrode
prepared by the standard method
(1) Joly, S.; Kane, R.; Radzilowski, L.; Wang, T.; Wu, A.; Cohen, R. E.; Thomas, E.
L.; Rubner, M. F. Langmuir 2000, 16, 1354.
(2) Polcaro, A.; Palmas, S.; Dernini, S. Ind. Eng. Chem. Res. 1993, 32, 1315.
(3) Pattabiraman, R., Applied Catalysis A. 1997, 153, 9.1.
Cyclic voltammetry shows the typical response of a polycrystalline Pd electrode3. The
anodic hydrogen peak is completely suppressed in the presence of acetophenone which
confirms the electrocatalytic activity. These properties were tested in batch process and
followed by HPLC. Complete reduction of acetophenone to ethyl benzene with a
current efficiency of 84% has been observed. In addition, the electrocatalytic
performance was compared with that of an electrode bearing Pd microcrystals prepared
by direct electroreduction of Pd(II) salts2,3 on the carbon surface resulting in a
reduction rate per mole of Pd ten-fold faster than for the microcrystalline Pd electrode
prepared by the standard method
(1) Joly, S.; Kane, R.; Radzilowski, L.; Wang, T.; Wu, A.; Cohen, R. E.; Thomas, E.
L.; Rubner, M. F. Langmuir 2000, 16, 1354.
(2) Polcaro, A.; Palmas, S.; Dernini, S. Ind. Eng. Chem. Res. 1993, 32, 1315.
(3) Pattabiraman, R., Applied Catalysis A. 1997, 153, 9.3. The
anodic hydrogen peak is completely suppressed in the presence of acetophenone which
confirms the electrocatalytic activity. These properties were tested in batch process and
followed by HPLC. Complete reduction of acetophenone to ethyl benzene with a
current efficiency of 84% has been observed. In addition, the electrocatalytic
performance was compared with that of an electrode bearing Pd microcrystals prepared
by direct electroreduction of Pd(II) salts2,3 on the carbon surface resulting in a
reduction rate per mole of Pd ten-fold faster than for the microcrystalline Pd electrode
prepared by the standard method
(1) Joly, S.; Kane, R.; Radzilowski, L.; Wang, T.; Wu, A.; Cohen, R. E.; Thomas, E.
L.; Rubner, M. F. Langmuir 2000, 16, 1354.
(2) Polcaro, A.; Palmas, S.; Dernini, S. Ind. Eng. Chem. Res. 1993, 32, 1315.
(3) Pattabiraman, R., Applied Catalysis A. 1997, 153, 9.2,3 on the carbon surface resulting in a
reduction rate per mole of Pd ten-fold faster than for the microcrystalline Pd electrode
prepared by the standard method
(1) Joly, S.; Kane, R.; Radzilowski, L.; Wang, T.; Wu, A.; Cohen, R. E.; Thomas, E.
L.; Rubner, M. F. Langmuir 2000, 16, 1354.
(2) Polcaro, A.; Palmas, S.; Dernini, S. Ind. Eng. Chem. Res. 1993, 32, 1315.
(3) Pattabiraman, R., Applied Catalysis A. 1997, 153, 9.Langmuir 2000, 16, 1354.
(2) Polcaro, A.; Palmas, S.; Dernini, S. Ind. Eng. Chem. Res. 1993, 32, 1315.
(3) Pattabiraman, R., Applied Catalysis A. 1997, 153, 9.Ind. Eng. Chem. Res. 1993, 32, 1315.
(3) Pattabiraman, R., Applied Catalysis A. 1997, 153, 9.Applied Catalysis A. 1997, 153, 9.