Synthesis and characterization of Mn-MCM-41 and Zr-Mn-MCM-41

M. Selvaraj, P. K. Sinha, K. Lee, I. Ahn, A. Pandurangan, T. G. Lee

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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 languageEnglish
Pages (from-to)139-149
Number of pages11
JournalMicroporous and Mesoporous Materials
Volume78
Issue number2-3
DOIs
Publication statusPublished - 2005 Mar 1

Fingerprint

manganese ions
Multicarrier modulation
absorbents
synthesis
Manganese
stilbene
porosity
thermal analysis
ions
Zirconium
Ions
silicon dioxide
nitrogen
transmission electron microscopy
oxidation
scanning electron microscopy
Mesoporous materials
adsorption
epoxidation
Molecular sieves

All Science Journal Classification (ASJC) codes

  • Chemistry(all)
  • Materials Science(all)
  • Condensed Matter Physics
  • Mechanics of Materials

Cite this

Selvaraj, M. ; Sinha, P. K. ; Lee, K. ; Ahn, I. ; Pandurangan, A. ; Lee, T. G. / Synthesis and characterization of Mn-MCM-41 and Zr-Mn-MCM-41. In: Microporous and Mesoporous Materials. 2005 ; Vol. 78, No. 2-3. pp. 139-149.
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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).",
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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 journalArticle

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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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