Laboratory Real-Time and In Situ Monitoring of Mechanochemical Milling Reactions by Raman Spectroscopy

被引：165

作者：

Gracin, Davor ^{[1
]}

Strukil, Vjekoslav ^{[1
]}

Friscic, Tomislav ^{[2
,3
]}

Halasz, Ivan ^{[1
]}

Uzarevic, Krunoslav ^{[1
]}

机构：

[1] Rudjer Boskovic Inst, Zagreb 10000, Croatia

[2] McGill Univ, Dept Chem, Montreal, PQ, Canada

[3] McGill Univ, Ctr Green Chem & Catalysis, Montreal, PQ, Canada

来源：

ANGEWANDTE CHEMIE-INTERNATIONAL EDITION | 2014年 / 53卷 / 24期

关键词：

in situ techniques; liquid-assisted grinding; mechanochemistry; Raman spectroscopy; reaction mechanisms; METAL-ORGANIC FRAMEWORKS; COCRYSTAL FORMATION; ACETONITRILE; REACTIVITY; MECHANISM; SOLVENT; TOOL;

D O I：

10.1002/anie.201402334

中图分类号：

O6 [化学];

学科分类号：

0703 ;

摘要：

Mechanistic understanding of mechanochemical reactions is sparse and has been acquired mostly by stepwise ex situ analysis. We describe herein an unprecedented laboratory technique to monitor the course of mechanochemical transformations at the molecular level in situ and in real time by using Raman spectroscopy. The technique, in which translucent milling vessels are used that enable the collection of a Raman scattering signal from the sample as it is being milled, was validated on mechanochemical reactions to form coordination polymers and organic cocrystals. The technique enabled the assessment of the reaction dynamics and course under different reaction conditions as well as, for the first time, direct insight into the behavior of liquid additives during liquid-assisted grinding.

引用

页码：6193 / 6197

页数：5

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