Ozonolysis in Flow Using Capillary Reactors
Ozonolysis in Flow Using Capillary Reactors
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使用毛细管反应器进行流动臭氧分解
DOI：
10.1021/op200036d
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发表时间：
2011
影响因子：
3.4
通讯作者：
Roydhouse M
中科院分区：
文献类型：
--
作者：
Roydhouse M
正癸烯与臭氧的反应和随后形成的臭氧化物的淬灭在流动条件下使用配备有冷却流动池的标准Vapourtec流动系统进行。反应连续进行，并在环形流动状态内的圆形横截面通道。典型的液体流速为0.25-1 mL min-1，气体流速为25-100 mL min-1，反应器体积为0.07-10 mL，由1 mm ID PFA管形成。反应温度为-10 °C。流动并不总是平滑的，同时观察到液膜中的波动和气核中的液滴。液体停留时间被发现是独立的气体流速和增加，随着液体流速的降低。底物在臭氧分解反应器中的停留时间在1和80 s之间，并且完全转化可以在0.01 s的停留时间内实现。两种常见的还原剂，亚磷酸三乙酯和三苯基膦，被检查为它们在流动条件下的适用性。三苯基膦实现了更快的中间体臭氧化物的还原，导致大于10：1的选择性的醛超过相应的酸。冷却系统提供了对高度放热的反应系统的安全和有效的控制。该系统的配置允许生产的化学显着的量（1.8克h-1在1.3臭氧当量），在任何时候都存在最少量的臭氧化物。
Reactions ofn-decene with ozone and subsequent quenching of the formed ozonides were carried out under flow conditions using the standard Vapourtec flow system equipped with a cooled flow cell. The reactions were performed continuously and in the annular flow regime within the circular cross-section channels. Typical flow rates were 0.25–1 mL min–1for liquid and 25–100 mL min–1for gas, reactor volumes were 0.07–10 mL formed of 1 mm ID PFA tubing. The reaction temperature was −10 °C. The flow was not always smooth, while waves in the liquid film and droplets in the gas core were observed. Liquid residence times were found to be independent of gas flow rates and increasing with decreasing liquid flow rates. Substrate residence times in the ozonolysis reactor ranged between 1 and 80 s, and complete conversion could be achieved at ∼1 s residence time. Two common reductants, triethylphosphite and triphenylphosphine, were examined as to their suitability under flow conditions. Triphenylphosphine achieved faster reduction of the intermediate ozonides, resulting in a greater than 10:1 selectivity for the aldehyde over the corresponding acid. The cooling system provided a safe and efficient control of the highly exothermic reaction system. The configuration of the system allowed the production of chemically significant amounts (1.8 g h–1at 1.3 ozone equivalents), with minimal amounts of ozonides present at any time.
减少三苯基膦臭氧取代苯乙烯的电影研究
DOI：
--
发表时间：
1970
期刊：
影响因子：
--
作者：
J. Carles;S. Fliszár
通讯作者：
S. Fliszár
DOI：
--
发表时间：
1972
期刊：
影响因子：
--
作者：
E. Moeck;J. W. Stachiewicz
通讯作者：
J. W. Stachiewicz