Reaction Mechanism and in Situ ATR Spectroscopic Studies of the 1-Decene Ozonolysis in Micro- and Semibatch Reactors
Reaction Mechanism and in Situ ATR Spectroscopic Studies of the 1-Decene Ozonolysis in Micro- and Semibatch Reactors
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DOI：
10.1021/ie900726s
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发表时间：
2010-01
影响因子：
4.2
通讯作者：
N. Steinfeldt;U. Bentrup;K. Jähnisch
中科院分区：
文献类型：
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作者：
N. Steinfeldt;U. Bentrup;K. Jähnisch
在降膜式微反应器和半间歇式反应器中，采用不同的溶剂（CH_2Cl_2、CH_3OH或两者的混合物）对1-癸烯（1）进行了臭氧化反应。臭氧分解的主要产物为3-辛基-1，2，4-三恶茂烷（7）和1-过氧氢-1-甲氧基壬烷（8）。在这两种情况下，选择性都高于70%，并且几乎不受1-癸烯转化率和反应温度的影响。臭氧分解主要通过将初级臭氧化物裂解成长链羰基氧化物（6）和甲醛（4）来进行。除了离线分析，原位ATR-FTIR光谱测量使用金刚石ATR探针被应用于跟踪反应进程。特征IR谱带的积分强度与从气相色谱/高效液相色谱分析获得的定量结果良好相关。因此，原位ATR被证明是一种快速和实时监测液相反应的合适方法，即使在存在…
The ozonolysis of 1-decene (1) was performed in a falling film microreactor and in a semibatch reactor using different solvents (CH2Cl2, CH3OH, or a mixture of both). The main products of ozonolysis were 3-octyl-1,2,4-trioxolane (7) in CH2Cl2 and 1-hydroperoxy-1-methoxynonane (8) in CH3OH or in a CH2Cl2/CH3OH mixture. In both cases the selectivities were higher than 70% and almost independent of 1-decene conversion and reaction temperature. The ozonolysis proceeds mainly via the cleavage of the primary ozonide into the long-chain carbonyl oxide (6) and formaldehyde (4). Besides off-line analysis in situ ATR-FTIR spectroscopic measurements using a diamond ATR probe were applied to follow the reaction progress. Integral intensities of characteristic IR bands correlate well with quantitative results obtained from gas chromatography/high-performance liquid chromatography analysis. Thus, in situ ATR proved to be a suitable method for fast and real-time monitoring of liquid-phase reactions even in the presence ...