Laser-supported high-temperature MAS NMR for time-resolved in situ studies of reaction steps in heterogeneous catalysis
Laser-supported high-temperature MAS NMR for time-resolved in situ studies of reaction steps in heterogeneous catalysis
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DOI：
10.1016/0926-2040(95)01214-1
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发表时间：
1996-04-01
影响因子：
3.2
通讯作者：
Wolf, I
中科院分区：
文献类型：
--
作者：
Ernst, H;Freude, D;Wolf, I
通过激光束，含有各种吸附分子的沸石样品的温度从室温快速改变（15 秒内）至 600 K。氮化硼容器中密封玻璃安瓿的位置降低了样品中的温度梯度并避免了激光诱发的反应。该技术有助于对 60 秒内发生的高温反应进行时间依赖性魔角旋转 (MAS) 核磁共振波谱分析。负载完全氘化分子的沸石氢形式的 H-D 交换、甲醇到汽油的转化以及沸石中的催化乙苯歧化反应均通过 C-13 和 H-1 MAS NMR 通过“停止和运行”方法进行监测。
The temperature of zeolite samples containing various adsorbed molecules was rapidly changed (within 15 s) from room temperature to 600 K by means of a laser beam. The location of the sealed glass ampoule in a boron nitride container decreases the temperature gradient in the sample and avoids laser-induced reactions. The technique facilitates time-dependent magic-angle-spinning (MAS) NMR spectroscopy of high-temperature reactions which take place within 60 s. The H-D exchange in the hydrogen form of zeolites loaded with fully deuterated molecules, the methanol-to-gasoline conversion and the catalytic ethylbenzene disproportionation in zeolites were monitored by C-13 and H-1 MAS NMR by means of a ''stop and go'' method.