Abstract
Mesoporous silica molecular sieves MCM-41 containing zirconium and manganese ions (Zr-Mn-MCM-41) with Si/(Zr+Mn) ratio equal to 49, 98, 147, 196, 262 and 327 and only manganese ions with Si/Mn ratio equal to 15, 31, 46, 61, 82 and 102 respectively, were synthesized under hydrothermal conditions using cetyltrimethylammonium (CTMA+) surfactants as template in the absence of auxiliary organics. The mesoporous materials, viz. Zr-Mn-MCM-41 and Mn-MCM-41 were characterized using several techniques, e.g. ICP-AES, XRD, FTIR, Nitrogen adsorption, TG/DTA, ESR, UV-Vis/DRS, SEM and TEM. ICP-AES studies indicated the content of zirconium and manganese in the mesoporous materials. XRD studies indicated that the materials had the standard MCM-41 structure. FTIR studies showed that zirconium and manganese ions were incorporated into the hexagonal mesoporous structure of Zr-Mn-MCM-41 and Mn-MCM-41. The thermal stability of the as-synthesized materials was studied using TG/DTA. Nitrogen adsorption was used to determine specific surface area, pore diameter, pore volume and wall thickness in the calcined Zr-Mn-MCM-41 and Mn-MCM-41 mesoporous molecular sieves. The incorporated of zirconium and manganese ions oxidation state was determined by ESR and UV-Vis/DRS. The morphology of Zr-Mn-MCM-41 and Mn-MCM-41 materials was determined by SEM. The inference that the Zr-Mn-MCM-41 and Mn-MCM-41 mesoporous materials had uniform pore size was obtained by TEM studies. The incorporated metal ions as Zr4+, Mn2+ and Mn3+ in Zr-Mn-MCM-41 are coordinated to Si(IV) by tetrahedral, disordered octahedral and tetrahedral environments respectively. The zirconium and manganese ions are homogenously dispersed on the inside silica surface of the Zr-Mn-MCM-41, but only the manganese ion is not homogenously dispersed on the inside surface of the Mn-MCM-41 under hydrothermal conditions. Thus the Zr-Mn-MCM-41 mesoporous molecular sieves are more useful for oxidation of olefin reaction with TBHP, e.g., in the epoxidation of frans-stilbene, frans-stilbene-oxide (84.58%) was found to be the highest in the presence of Zr-Mn-MCM-41(49).
| Original language | English |
|---|---|
| Pages (from-to) | 139-149 |
| Number of pages | 11 |
| Journal | Microporous and Mesoporous Materials |
| Volume | 78 |
| Issue number | 2-3 |
| DOIs | |
| Publication status | Published - 2005 Mar 1 |
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All Science Journal Classification (ASJC) codes
- Chemistry(all)
- Materials Science(all)
- Condensed Matter Physics
- Mechanics of Materials
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Synthesis and characterization of Mn-MCM-41 and Zr-Mn-MCM-41. / Selvaraj, M.; Sinha, P. K.; Lee, K.; Ahn, I.; Pandurangan, A.; Lee, T. G.
In: Microporous and Mesoporous Materials, Vol. 78, No. 2-3, 01.03.2005, p. 139-149.Research output: Contribution to journal › Article
TY - JOUR
T1 - Synthesis and characterization of Mn-MCM-41 and Zr-Mn-MCM-41
AU - Selvaraj, M.
AU - Sinha, P. K.
AU - Lee, K.
AU - Ahn, I.
AU - Pandurangan, A.
AU - Lee, T. G.
PY - 2005/3/1
Y1 - 2005/3/1
N2 - Mesoporous silica molecular sieves MCM-41 containing zirconium and manganese ions (Zr-Mn-MCM-41) with Si/(Zr+Mn) ratio equal to 49, 98, 147, 196, 262 and 327 and only manganese ions with Si/Mn ratio equal to 15, 31, 46, 61, 82 and 102 respectively, were synthesized under hydrothermal conditions using cetyltrimethylammonium (CTMA+) surfactants as template in the absence of auxiliary organics. The mesoporous materials, viz. Zr-Mn-MCM-41 and Mn-MCM-41 were characterized using several techniques, e.g. ICP-AES, XRD, FTIR, Nitrogen adsorption, TG/DTA, ESR, UV-Vis/DRS, SEM and TEM. ICP-AES studies indicated the content of zirconium and manganese in the mesoporous materials. XRD studies indicated that the materials had the standard MCM-41 structure. FTIR studies showed that zirconium and manganese ions were incorporated into the hexagonal mesoporous structure of Zr-Mn-MCM-41 and Mn-MCM-41. The thermal stability of the as-synthesized materials was studied using TG/DTA. Nitrogen adsorption was used to determine specific surface area, pore diameter, pore volume and wall thickness in the calcined Zr-Mn-MCM-41 and Mn-MCM-41 mesoporous molecular sieves. The incorporated of zirconium and manganese ions oxidation state was determined by ESR and UV-Vis/DRS. The morphology of Zr-Mn-MCM-41 and Mn-MCM-41 materials was determined by SEM. The inference that the Zr-Mn-MCM-41 and Mn-MCM-41 mesoporous materials had uniform pore size was obtained by TEM studies. The incorporated metal ions as Zr4+, Mn2+ and Mn3+ in Zr-Mn-MCM-41 are coordinated to Si(IV) by tetrahedral, disordered octahedral and tetrahedral environments respectively. The zirconium and manganese ions are homogenously dispersed on the inside silica surface of the Zr-Mn-MCM-41, but only the manganese ion is not homogenously dispersed on the inside surface of the Mn-MCM-41 under hydrothermal conditions. Thus the Zr-Mn-MCM-41 mesoporous molecular sieves are more useful for oxidation of olefin reaction with TBHP, e.g., in the epoxidation of frans-stilbene, frans-stilbene-oxide (84.58%) was found to be the highest in the presence of Zr-Mn-MCM-41(49).
AB - Mesoporous silica molecular sieves MCM-41 containing zirconium and manganese ions (Zr-Mn-MCM-41) with Si/(Zr+Mn) ratio equal to 49, 98, 147, 196, 262 and 327 and only manganese ions with Si/Mn ratio equal to 15, 31, 46, 61, 82 and 102 respectively, were synthesized under hydrothermal conditions using cetyltrimethylammonium (CTMA+) surfactants as template in the absence of auxiliary organics. The mesoporous materials, viz. Zr-Mn-MCM-41 and Mn-MCM-41 were characterized using several techniques, e.g. ICP-AES, XRD, FTIR, Nitrogen adsorption, TG/DTA, ESR, UV-Vis/DRS, SEM and TEM. ICP-AES studies indicated the content of zirconium and manganese in the mesoporous materials. XRD studies indicated that the materials had the standard MCM-41 structure. FTIR studies showed that zirconium and manganese ions were incorporated into the hexagonal mesoporous structure of Zr-Mn-MCM-41 and Mn-MCM-41. The thermal stability of the as-synthesized materials was studied using TG/DTA. Nitrogen adsorption was used to determine specific surface area, pore diameter, pore volume and wall thickness in the calcined Zr-Mn-MCM-41 and Mn-MCM-41 mesoporous molecular sieves. The incorporated of zirconium and manganese ions oxidation state was determined by ESR and UV-Vis/DRS. The morphology of Zr-Mn-MCM-41 and Mn-MCM-41 materials was determined by SEM. The inference that the Zr-Mn-MCM-41 and Mn-MCM-41 mesoporous materials had uniform pore size was obtained by TEM studies. The incorporated metal ions as Zr4+, Mn2+ and Mn3+ in Zr-Mn-MCM-41 are coordinated to Si(IV) by tetrahedral, disordered octahedral and tetrahedral environments respectively. The zirconium and manganese ions are homogenously dispersed on the inside silica surface of the Zr-Mn-MCM-41, but only the manganese ion is not homogenously dispersed on the inside surface of the Mn-MCM-41 under hydrothermal conditions. Thus the Zr-Mn-MCM-41 mesoporous molecular sieves are more useful for oxidation of olefin reaction with TBHP, e.g., in the epoxidation of frans-stilbene, frans-stilbene-oxide (84.58%) was found to be the highest in the presence of Zr-Mn-MCM-41(49).
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UR - http://www.scopus.com/inward/citedby.url?scp=13444253755&partnerID=8YFLogxK
U2 - 10.1016/j.micromeso.2004.10.004
DO - 10.1016/j.micromeso.2004.10.004
M3 - Article
AN - SCOPUS:13444253755
VL - 78
SP - 139
EP - 149
JO - Microporous and Mesoporous Materials
JF - Microporous and Mesoporous Materials
SN - 1387-1811
IS - 2-3
ER -