非均相羰基氧化合成碳酸二苯酯反应液组分的分析

Analysis of Reaction Products of Heterogeneous Catalytic Synthesis of Diphenyl Carbonate

通过色质联用仪对非均相催化一步合成碳酸二苯酯(DPC)过程中的反应液的主要产物及副产物进行了定性分析,其结果发现该反应的主要副产物为苯氧基丙酸和4-苯氧基苯酚以及四丁基铵盐;用气相色谱外标法对反应液中的DPC进行了定量分析,并通过回归法得到了定量分析DPC的计算方程式,实验证明该方程在DPC的浓度小于10%范围内比较可靠。

The products and byproducts of the‘one_step’heterogeneous catalytic synthesis of diphenyl carbonate were identified by GC-MS.The main side_products has been found to be3_phenoxypropanonic acid,4_phenoxy_ phenol and tetrabutylammonium salt(chloride,bromide and cyanide).Quantitative determination of diphenyl carbonate was carried out with GC by external standard method.A linear regression equation for DPC weight content(w)versus its peak area(A)was obtained:w=-0.25158+1.19274×10 -4 A.As shown by our testing results,the proposed method can be applied to the quantitative determination of DPC,provided the DPC weight content is lower than10%.