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In Situ Investigations of Mechanochemical One‐Pot Syntheses
Author(s) -
Kulla Hannes,
Haferkamp Sebastian,
Akhmetova Irina,
Röllig Mathias,
Maierhofer Christiane,
Rademann Klaus,
Emmerling Franziska
Publication year - 2018
Publication title -
angewandte chemie international edition
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 5.831
H-Index - 550
eISSN - 1521-3773
pISSN - 1433-7851
DOI - 10.1002/anie.201800147
Subject(s) - crystallization , in situ , synchrotron , raman spectroscopy , chemistry , kinetics , knoevenagel condensation , chemical engineering , materials science , thermodynamics , catalysis , organic chemistry , physics , quantum mechanics , nuclear physics , optics , engineering
We present an in situ triple coupling of synchrotron X‐ray diffraction with Raman spectroscopy, and thermography to study milling reactions in real time. This combination of methods allows a correlation of the structural evolution with temperature information. The temperature information is crucial for understanding both the thermodynamics and reaction kinetics. The reaction mechanisms of three prototypical mechanochemical syntheses, a cocrystal formation, a C−C bond formation (Knoevenagel condensation), and the formation of a manganese‐phosphonate, were elucidated. Trends in the temperature development during milling are identified. The heat of reaction and latent heat of crystallization of the product contribute to the overall temperature increase. A decrease in temperature occurs via release of, for example, water as a by‐product. Solid and liquid intermediates are detected. The influence of the mechanical impact could be separated from temperature effects caused by the reaction.