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Synthesis and Characterization of Silanol Derivative of Keggin Tungstocobaltate[CoW11O40(SiOH)2]5-(PDF)

《南京师大学报(自然科学版)》[ISSN:1001-4616/CN:32-1239/N]

Issue:
2013年03期
Page:
48-52
Research Field:
化学
Publishing date:

Info

Title:
Synthesis and Characterization of Silanol Derivative of Keggin Tungstocobaltate[CoW11O40(SiOH)2]5-
Author(s):
Zhang JianpingYang Chun
School of Chemistry and Materials Science,Nanjing Normal University,Nanjing 210097,China
Keywords:
tungstocobaltatesilanol substitutedKeggin structuresynthesis and characterization
PACS:
O611.4
DOI:
-
Abstract:
The Keggin-type silanol substituted tungstocobaltate[CoW11O40(SiOH)2]5- was synthesized for the first time by using CoW11 and TEOS as start materials in an ethanol-water mixing solvent.The structure and composition of the products were characterized by IR,UV-vis,TG-DTA and elemental analysis techniques.The results showed that two Si atoms were inserted into the vacancy of CoW11 and a Si-O-Si bridge was formed between two Si atoms.The symmetry of the product is between saturated and vacant Keggin structure.Moreover,the effect of synthesis conditions on the product was also investigated.It is demonstrated that the pH and the volume ratio of ethanol to water greatly influence the yield and the purity of the product.A proper matching of acidity and ethanol dosage is necessary.The product with good yield and high purity was obtained under pH=1 and VEtOH:VH20=2:1.

References:

[1] Zhang R F,Yang C.A novel polyoxometalate-functionalized mesoporous hybrid silica:synthesis and characterization[J].J Mater Chem,2008,18(23):2 691-2 703.
[2]王金娥,杨春.二次嫁接法合成多金属氧酸盐/介孔分子筛杂化材料[J].化学学报,2009,67(4):271-275.
[3]Luo X J,Yang C.Photochromic ordered mesoporous hybrid materials based on covalently grafted polyoxometalates[J].Phys Chem Chem Phys,2011,13(17):7 892-7 902.
[4]Knoth W H.Derivatives of heteropolyanions.1.organic derivatives of W12SiO404-,W12PO403- and Mo12SiO404-[J].J Am Chem Soc,1979,101(3):759-760.
[5]Ammari N,Hervé G,Thouvenot R.A new class of organosilyl derivatives of polyoxoanions:attachment of alkyl- and arylsilyl groups on trivacant tungstosilicate[J].New J Chem,1991,15(8/9):607-608.
[6]Agustin D,Dallety J,Coelho C,et al.Synthesis,characterization and study of the chromogenic properties of the hybrid polyoxometalates[PW11O39(SiR)2O]3-(R=Et,(CH2)nCH=CH2(n=0,1,4),CH2CH2SiEt3,CH2CH2SiMe2Ph)[J].J Organometallic Chem,2007,692(4):746-754.
[7]Baker L C W,McCutcheon T P.Heteropoly salts containing cobalt and hexavalent tungsten in the anion[J].J Am Chem Soc,1956,78(18):4 503-4 510.
[8]Bas-Serra J,Todorut I,Casañ-Pastor N,et al.Synthesis and characterization new Keggin based structure tungstocobaltates:K9[Co3+W11O39]and vanadium derivatives,K8[Co2+W11V4+O40],K7[Co2+W11V5+O40],and K6[Co3+W11V5+O40][J].Synth React Inorg Met-Org Chem,1995,25(6):869-882.
[9]余锡宾,吴虹.正硅酸乙酯的水解、缩合过程研究[J].无机材料学报,1996,11(4):703-707.
[10]Nomiya K,Kobayashi R,Miwa M.An improved preparation and characterization of tetrahedral Co and Co complexes with dodecatungstate as the tetrahedral ligand[J].Bull Chem Soc Jpn,1983,56(8):2 272-2 275.
[11]Judeinstein P,Deprun C,Nadjo L.Synthesis and multispectroscopic characterization of organically modified polyoxometalates[J].J Chem Soc Dalton Trans,1991(8):1 991-1 997.
[12]Kojima K,Matsuda J,Kojima N,et al.Optical and ESR spectra for high-spin tetrahedral complexes of Co(Ⅲ)and Co(Ⅱ)in Keggin-structure heteropolytungstate[J].Bull Chem Soc Jpn,1987,60(9):3 213-3 217.
[13]Kojima K,Matsuda J.Absorption spectra of tetrahedral Co(Ⅲ)and Co(Ⅱ)complexes in heteropolytungstates[J].Bull Chem Soc Jpn,1985,58(3):821-825.
[14]王恩波,刘连利,沈恩洪,等.含2A主族元素杂多钨酸盐的合成及性质[J].应用化学,1991,8(5):13-16.

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Last Update: 2013-09-30