Preparation and Characterization of Pd Modified TiO 2 Nanofiber Catalyst for Carbon–Carbon Coupling Heck Reaction
TiO 2 fibers were prepared through electrospinning of poly methyl methacrylate (PMMA) and titanium isopropoxide (TIP) solution followed by calcination of fibers in air at 500°C. Cetyltrimethylammonium bromide (CTAB) protected palladium nanoparticles (Pd NPs) prepared through reduction method were su...
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| Published in | Journal of nanomaterials Vol. 2017; pp. 1 - 13 |
|---|---|
| Main Authors | , , , , , |
| Format | Journal Article |
| Language | English |
| Published |
2017
|
| Online Access | Get full text |
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| Abstract | TiO
2
fibers were prepared through electrospinning of poly methyl methacrylate (PMMA) and titanium isopropoxide (TIP) solution followed by calcination of fibers in air at 500°C. Cetyltrimethylammonium bromide (CTAB) protected palladium nanoparticles (Pd NPs) prepared through reduction method were successfully adsorbed on the TiO
2
nanofibers (NF). Combined studies of X-ray diffraction (XRD), scanning electron microscope (SEM), and transmission electron microscope (TEM) indicated that the synthesized Pd/TiO
2
had anatase. BET indicated that the synthesized TiO
2
and Pd/TiO
2
had a surface area of 53.4 and 43.4 m
2
/g, respectively. The activity and selectivity of 1 mol% Pd/TiO
2
in the Heck reaction have been investigated towards the Mizoroki-Heck carbon–carbon cross-coupling of bromobenzene (ArBr) and styrene. Temperature, time, solvent, and base were optimized and catalyst was recycled thrice.
1
H NMR and
13
C NMR indicated that stilbene, a known compound from literature, was obtained in various Heck reactions at temperatures between 100°C and 140°C but the recyclability was limited due to some palladium leaching and catalyst poisoning which probably arose from some residual carbon from the polymer. The catalyst was found to be highly active under air atmosphere with reaction temperatures up to 140°C. Optimized reaction condition resulted in 89.7% conversions with a TON of 1993.4 and TOF value of 332.2 hr
−1
. |
|---|---|
| AbstractList | TiO
2
fibers were prepared through electrospinning of poly methyl methacrylate (PMMA) and titanium isopropoxide (TIP) solution followed by calcination of fibers in air at 500°C. Cetyltrimethylammonium bromide (CTAB) protected palladium nanoparticles (Pd NPs) prepared through reduction method were successfully adsorbed on the TiO
2
nanofibers (NF). Combined studies of X-ray diffraction (XRD), scanning electron microscope (SEM), and transmission electron microscope (TEM) indicated that the synthesized Pd/TiO
2
had anatase. BET indicated that the synthesized TiO
2
and Pd/TiO
2
had a surface area of 53.4 and 43.4 m
2
/g, respectively. The activity and selectivity of 1 mol% Pd/TiO
2
in the Heck reaction have been investigated towards the Mizoroki-Heck carbon–carbon cross-coupling of bromobenzene (ArBr) and styrene. Temperature, time, solvent, and base were optimized and catalyst was recycled thrice.
1
H NMR and
13
C NMR indicated that stilbene, a known compound from literature, was obtained in various Heck reactions at temperatures between 100°C and 140°C but the recyclability was limited due to some palladium leaching and catalyst poisoning which probably arose from some residual carbon from the polymer. The catalyst was found to be highly active under air atmosphere with reaction temperatures up to 140°C. Optimized reaction condition resulted in 89.7% conversions with a TON of 1993.4 and TOF value of 332.2 hr
−1
. |
| Author | Onindo, Charles O. Makhubela, Banothile C. E. Nyangasi, Leah O. Ngila, Jane C. Ngigi, Eric M. Andala, Dickson M. |
| Author_xml | – sequence: 1 givenname: Leah O. orcidid: 0000-0002-6080-9616 surname: Nyangasi fullname: Nyangasi, Leah O. organization: Chemistry Department, Kenyatta University, P.O. Box 43844-00100, Nairobi, Kenya, Natural Science Department, Catholic University of Eastern Africa, P.O. Box 62157-00200, Nairobi, Kenya – sequence: 2 givenname: Dickson M. surname: Andala fullname: Andala, Dickson M. organization: Chemistry Department, Multimedia University of Kenya, P.O. Box 30305-00100, Nairobi, Kenya – sequence: 3 givenname: Charles O. surname: Onindo fullname: Onindo, Charles O. organization: Chemistry Department, Kenyatta University, P.O. Box 43844-00100, Nairobi, Kenya – sequence: 4 givenname: Jane C. surname: Ngila fullname: Ngila, Jane C. organization: Department of Applied Chemistry, University of Johannesburg, P.O. Box 17011, Corner Beit and Nind Street, Doornfontein, Johannesburg 2028, South Africa – sequence: 5 givenname: Banothile C. E. surname: Makhubela fullname: Makhubela, Banothile C. E. organization: Department of Chemistry, University of Johannesburg, P.O. Box 17011, Kingsway Campus, Auckland Park 2006, South Africa – sequence: 6 givenname: Eric M. surname: Ngigi fullname: Ngigi, Eric M. organization: Department of Applied Chemistry, University of Johannesburg, P.O. Box 17011, Corner Beit and Nind Street, Doornfontein, Johannesburg 2028, South Africa |
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| CitedBy_id | crossref_primary_10_3390_membranes12020236 crossref_primary_10_1016_j_inoche_2023_111035 crossref_primary_10_1016_j_molstruc_2024_139081 crossref_primary_10_1021_acsami_0c09106 crossref_primary_10_1039_D0NJ05032F crossref_primary_10_2174_1570193X16666190617160339 crossref_primary_10_1002_ente_202301063 crossref_primary_10_1007_s10853_020_05610_6 |
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