Linking Simultaneous In Situ WAXS/SAXS/Raman with Raman/ATR/UV-vis Spectroscopy: Comprehensive Insight into the Synthesis of Molybdate Catalyst Precursors

被引：29

作者：

Bentrup, Ursula ^{[1
]}

Radnik, Joerg ^{[1
]}

Armbruster, Udo ^{[1
]}

Martin, Andreas ^{[1
]}

Leiterer, Jork ^{[2
]}

Emmerling, Franziska ^{[2
]}

Brueckner, Angelika ^{[1
]}

机构：

[1] Univ Rostock, Leibniz Inst Katalyse eV, D-18059 Rostock, Germany

[2] Bundesanstalt Mat Forsch & Prufung, D-12489 Berlin, Germany

来源：

TOPICS IN CATALYSIS | 2009年 / 52卷 / 10期

关键词：

In situ; WAXS/SAXS; Raman; ATR; UV-vis; Mixed oxide catalyst; Synthesis; SELECTIVE OXIDATION; CRYSTALLIZATION; PROPANE; FTIR;

D O I：

10.1007/s11244-009-9309-y

中图分类号：

O69 [应用化学];

学科分类号：

081704 ;

摘要：

A new setup is presented which enables simultaneous wide- and small-angle X-ray scattering (WAXS/SAXS) and Raman spectroscopic experiments during the synthesis of Mo-based mixed oxide catalyst precursors at the mu-spot beamline at the Berliner Elektronenspeicherring-Gesellschaft fur Synchrotronstrahlung (BESSY). Furthermore, we report about the separate monitoring of the same reactions under comparable conditions by simultaneous combined ATR/UV-vis/Raman spectroscopic measurements. For testing the performance of both experimental setups two syntheses were described comprising the precipitation of metal molybdates by mixing solutions of metal nitrates and ammonium heptamolybdate. Additionally, the effect of H3PO4 admixture on precipitation was investigated. The combined evaluation of spectroscopic and WAXS/SAXS data allows the discrimination between different molybdate species appearing in solution and precipitate. Furthermore, these molybdate species could be assigned to separate phases of different crystallinity.

引用

页码：1350 / 1359

页数：10

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