苯酚液相氧化羰化反应产物的GC-MS分析

GC-MS Analysis of the Products from Liquid Phase Oxidative Carbonylation of Phenol

利用GC-MS对有机/无机杂化材料(OIH)负载氯化钯催化剂催化苯酚液相氧化羰化合成碳酸二苯酯(DPC)不同催化体系的产物及副产物进行了定性分析,用GC外标法对反应液进行了定量分析。分析结果表明,产物分布与催化体系组成有关。在PdCl2/OIH-Co(OAc)2-CH2Cl2体系中,生成的主要副产物为水杨酸苯酯、醋酸苯酯、p-溴化苯酚和三正丁基铵;PdCl2/OIH-Cu2O-THF体系副产物则较少,只有水杨酸苯酯和三正丁基铵生成。并在分析结果的基础上提出了副产物的生成机理。

The aimed products and byproducts from liquid phase oxidative carbonylation of phenol to diphenyl carbonate （DPC） with different catalytic systems were identified by GC-MS, and the quantitative determination was carried out by GC with external standard method. The results showed that the distribution of products was affected by the composition of the catalytic system. Phenyl salicylate, phenyl acetate, pbromophenols and tributylamine were detected in OIH-DACH-PdCl2-Co（OAc）2-CH2Cl2 catalytic system, and no phenyl acetate was detected in OIH-DACH-PdCl2-Cu2O-THF catalytic system. The possible mechanism of byproducts formation was also proposed.