• 제목/요약/키워드: $^{51}V$ NMR

검색결과 33건 처리시간 0.024초

Characterization by Solid-State $^51V$ NMRand X-ray Diffraction of Vanadium Oxide Supported on ZrO₂

  • 손종락;박만영;배영일
    • Bulletin of the Korean Chemical Society
    • /
    • 제17권3호
    • /
    • pp.274-278
    • /
    • 1996
  • Vanadium oxide-zirconia catalysts were prepared by dry impregnation of powdered Zr(OH)4 with aqueous solution of NH4VO3. The characterization of prepared catalysts was performed using 51V solid state NMR, XRD, and DSC. The addition of vanadium oxide up to 9 mol% to zirconia shifted the phase transitions of ZrO2 from amorphous to tetragonal toward higher temperatures due to the interaction between vanadium oxide and zirconia. On the basis of results of XRD and DSC, it is concluded that the content of V2O5 monolayer covering most of the available zirconia was 9 mol%. The crystalline V2O5 was observed only with the samples containing V2O5 content exceeding the formation of complete monolayer (9 mol%) on the surface of ZrO2.

Synthesis and Spectroscopic Characterization of Vanadium incorporated V-AlMCM-41 Molecular Sieves

  • Back, Gern-Ho;Yu, Jong-Sung;Lee, Hye-Young;Lee, Yong-Ill
    • 한국자기공명학회논문지
    • /
    • 제10권2호
    • /
    • pp.141-154
    • /
    • 2006
  • A solid-state reaction of $V_2O_5$ with AlMCM-41 followed by calcinations generated $V^{5+}$ species in the mesoporous materials. Dehydration results in the formation of a vanadyl species, $VO^{2+}$, that can be characterized by electron spin resonance (ESR). The chemical environment of the vanadium centers in V-AlMCM-41 was investigated by XRD, EDX, diffuse reflectance UV-VIS, ESR, $^{29}Si,\;^{27}Al,\;and\;^{51}V$ NMR. It was found that the vanadium species on the wall surface and inside the wall of the hexagonal tubular wall of the V-AlMCM-41 were completely oxidized to tetrahedral $V^{5+}$ and transformed to square pyramidal by additional coordination to water molecules upon hydration. The oxidized $V^{5+}$ species on the wall surfaces and inside the wall were also reversibly reduced to $VO^{2+}$ species or lower valences by thermal process.

  • PDF

$^{13}C$ and $^{51}V$ Nuclear Magnetic Resonance Studies of Vanadium(V) Complexes of Iminodiacetate Analogues

  • Lee, Man-Ho
    • Bulletin of the Korean Chemical Society
    • /
    • 제13권1호
    • /
    • pp.22-26
    • /
    • 1992
  • The solution structures of the vanadium(V) complexes of iminodiacetate analogues, such as iminodiacetate (IDA), methyliminodiacetate (MeIDA), ethyliminodiacetate (EtIDA), benzyliminodiacetate (BzIDA), pyridine-2,6-dicarboxylate (DPA), and 2-hydroxyethyliminodiacetate (HEIDA), have been studied by $^{13}C-$ and $^{51}V$-NMR spectroscopy. Assuming that the complexes have a $cis-VO_2$ core, IDA, MeIDA, EtIDA, and BzIDA act as facial tridentate ligands to form octahedral complexes, whereas DPA coordinates to $VO_2^+$ as a meridional tridentate. And one water molecule fulfills the remaining site to satisfy the coordination number of six. But HEIDA coordinates to $VO_2^+$ through one IDA moiety and one hydroxyl group, acting as a tetradenate.

주목 잎의 후라보노이드 배당체 (Flavonoid Glycosides from Needles of Taxus cuspidata(Taxaceae))

  • 함연호;박완근;한상섭;배영수
    • Journal of the Korean Wood Science and Technology
    • /
    • 제25권2호
    • /
    • pp.45-51
    • /
    • 1997
  • 주목 잎을 채취하여 건조하고 아세톤-물 (7 : 3, v/v) 의 혼합액으로 추출한 후 에틸아세테이트 및 수용성 부분으로 분리하고 Sephadex-LH 20으로 충진한 칼럼을 이용하여 2개의 flavan 단량체와 2개의 후라보노이드 배당체를 단리하였다. 에틸아세테이트용성 추출물은 대부분 (+)-catechin 과 (-)-epicatechin으로 구성되어 있었으며 수용성 부분에서는 quercetin-3-0-arabinopyranosyl-($1"'{\rightarrow}6"$)-${\beta}$-D-glucoside와 quercetin-3-O-rutinoside 인 두 개의 탄수화물로 구성된 배당체를 분리하였으며 주목에서는 이들 화합물은 아직 보고된 바가 없다. 이들의 구조결정을 위하여 박층크로마토그래피를 실시하고 $^1H$-NMR과 $^{13}C$-NMR 스펙트럼을 기존의 스펙트럼과 비교, 분석하여 정확한 구조를 규명하였다.

  • PDF

Solid state MAS NMR Investigation on the Local Structures of xV2O5-B2O3-yNa2O Glasses

  • Kim, Sun-Ha;Han, Oc-Hee;Kang, Jae-Pil;Song, Seung-Ki
    • Bulletin of the Korean Chemical Society
    • /
    • 제30권3호
    • /
    • pp.608-612
    • /
    • 2009
  • The local structures of the boron and vanadium sites in the ternary glass $xV_2O_5-B_2O_3-yNa_2O$ were studied by $^{11}B\;and\;^{51}V$ magic angle spinning (MAS) nuclear magnetic resonance (NMR). With increasing x, the mole ratios of the $BO_3\;and\;BO_4$ structures were enhanced, as were the quadrupole asymmetry parameters for the $BO_3$ structures, while the quadrupole coupling constants for the sites were reduced. However, the opposite trends were observed with increasing y, implying that $V_2O_5$ and $Na_2O$ play opposite roles. The $VO_4,\;VO_5\;and\;VO_6$ structures with all oxygens bonded to the vanadium neighbors were identified. Vanadiums bonded to the greater number of oxygens were more populated at higher contents of $Na_2O\;and\;V_2O_5$. In addition, the $VO_4$ structures with at least one oxygen bonded to boron instead of vanadium were detected at low $Na_2O$ contents. The electron densities of various vanadium oxide structures were affected by the weight densities and vanadium ion densities. The $VO_4$ structures were more likely to be vanadium oxide structures right next to $V4^{+}$ ions.

$^{13}C\;and\;^{51}V $ Nuclear Magnetic Resonance Studies of Vanadium (Ⅴ)-$\alpha$-Hydroxycarboxylate Complexes

  • Man-Ho Lee;In-Whan Kim
    • Bulletin of the Korean Chemical Society
    • /
    • 제14권5호
    • /
    • pp.557-561
    • /
    • 1993
  • The interaction of vanadium(V) with various a-hydroxycarboxylate ligands in aqueous solution at pH 3.2 have been studied by $^{51}V$ and $^{13}C$ NMR spectroscopies. From the results it is supposed that vanadates mainly form the octahedral complexes with lactate, 2-hydroxybutyrate, glycerate, and malate. While, vanadates form the trigonal-bipyramidal complexes with glycolate, tartarate, and 2-hydroxy-3-methylbutyrate, and tetrahedral complexes with pyruvate(diol), 2-hydroxyisobutyrate, and 2-hydroxy-3-methylbutyrate. The bipyramidal products are formed as monomeric compounds. The octahedral products are formed as dimeric compounds with no evidence for a significant proportion of the monomeric derivatives. The complexes are mainly formed through the coordination at the carboxylate and the 2-hydroxyl groups of the ligands.

Effect of V2O5 Modification in V2O5/TiO2-ZrO2 Catalysts on Their Surface Properties and Catalytic Activities for Acid Catalysis

  • Sohn, Jong-Rack;Lee, Cheul-Kyu
    • Bulletin of the Korean Chemical Society
    • /
    • 제28권12호
    • /
    • pp.2459-2465
    • /
    • 2007
  • V2O5/TiO2-ZrO2 catalyst modified with V2O5 was prepared by adding Ti(OH)4-Zr(OH)4 powder into an aqueous solution of ammonium metavanadate followed by drying and calcining at high temperatures. The characterization of prepared catalysts was performed using XRD, DSC, solid-state 51V NMR, and FTIR. In the case of calcination temperature of 500 oC, for the catalysts containing low loading V2O5 below 25 wt % vanadium oxide was in a highly dispersed state, while for catalysts containing high loading V2O5 equal to or above 25 wt % vanadium oxide was well crystallized due to the V2O5 loading exceeding the formation of monolayer on the surface of TiO2-ZrO2. The strong acid sites were formed through the bonding between dispersed V2O5 and TiO2-ZrO2. The larger the dispersed V2O5 amount, the higher both the acidity and catalytic activities for acid catalysis.