空气氧化二苯甲醇反应体系的分析

Determination of Diphenylcarbinol Conversion in its Air Oxidation

采用傅里叶变换红外光谱和氮气吸附方法对溶胶-凝胶技术包埋的催化剂进行了表征。利用薄层色谱法和高效液相色谱法定性、定量分析了空气氧化二苯甲醇合成二苯甲酮的反应。实验中所用高效液相色谱柱为ODS-C18反相柱,以甲醇与水(体积比为85/15)为流动相,采用254nm紫外光进行检测。探讨了流动相中有机相的比例及检测波长等因素对分离度和灵敏度的影响。实验结果表明,该方法操作简便、快速、可靠。其相对标准偏差为3 7%,线性相关系数为0 999,变异系数为1 65%。

Determination of diphenylcarbinol conversion in air oxidation by reversed phase high performance liquid -chromatography and TLC was described.Diphenylcarbinol was successfully separated on an ODS-C18 reversed -phase column(46 mm ×150 mm,10 μm) using methanol -water (85/15,volume ratio) as mobile phase at a flow rate of 1 ml/min and detected at 254 nm.Effects of concentration of mobile phase and detection wavelength on response and retention were studied.Relative standard deviation,linear correlation and variation coefficients were determined to be 0037%,0999%,and 165% respectively.The method was proved to be fast,accurate and reliable.Diphenylcarbinol conversion in air oxidation attained 9475%.FTIR characterization results showed oxidation catalyst Co(acac)2 was entrapped in the three -dimensional network of silica.