We present an approach towards the in situ solid state NMR monitoring of mechanochemical reactions in a ball mill. A miniaturized vibration ball mill is integrated into the measuring coil of a home-built solid state NMR probe, allowing for static solid state NMR measurements during the mechanochemical reaction within the vessel. The setup allows to quantitatively follow the product evolution of a prototypical mechanochemical reaction, the formation of zinc phenylphosphonate from zinc acetate and phenylphosphonic acid. MAS NMR investigations on the final reaction mixture confirmed a reaction yield of 89% in a typical example. Thus, NMR spectroscopy may in the future provide complementary information about reaction mechanisms of mechanochemical reactions and team up with other analytical methods which have been employed to follow reactions in situ, such as Raman spectroscopy or X-ray diffraction.

我们提出了一种就地方法在球磨机中进行机械化学反应的固态NMR监测。小型振动球磨机集成在家用固态NMR探针的测量线圈中，可在容器内进行机械化学反应期间进行静态固态NMR测量。该设置允许定量跟踪原型机械化学反应的产物演变，即由乙酸锌和苯基膦酸形成苯基膦酸锌。在典型实例中，对最终反应混合物的MAS NMR研究证实反应产率为89％。因此，NMR光谱法将来可能会提供有关机械化学反应的反应机理的补充信息，并与其他已用于现场追踪反应的分析方法合作，例如拉曼光谱或X射线衍射。