氯化磷酸二苯酯的合成和结构表征

以苯酚、三氯氧磷为原料,以无水三氯化铝为催化剂合成了氯化磷酸二苯酯;采用正交试验研究了反应温度、反应时间、催化剂用量和原料配比对反应收率的影响,确定了最佳工艺条件;并利用红外光谱和核磁共振谱表征了产物的结构.结果表明,影响反应收率的几种因素的排序为:反应温度>原料配比>催化剂用量>反应时间;最佳反应条件为:温度70℃、反应时间15h、原料配比(n苯酚∶n三氯氧磷)2∶1、催化剂用量0.8g(相对于苯酚的质量分数为4.25%).与此同时,采用加水后处理方法可以提高产品收率和可操作性.

Synthesis and structural characterization of diphenyl chlorophosphate

Diphenyl chlorophosphate（DPCP） was synthesized with phenol and phosphorus oxychloride as the raw materials and anhydrous aluminum trichloride as the catalyst.The effects of reaction temperature,reaction time,catalyst dosage,and raw material molar ratio on the yield were investigated by orthogonal test,and the optimal reaction condition was established accordingly.Besides,the structure of as-synthesized DPCP product was characterized by means of infrared spectrometry and nuclear magnetic resonance spectroscopy.Results indicate that,in terms of the effect on the yield,various factors can be ranked as reaction temperatureraw material molar ratiocatalyst dosagereaction time.The optimal reaction condition is suggested as reaction temperature of 70 ℃,reaction time of 15 h,raw material molar ratio（phenol to phosphorus oxychloride） of 2∶1,and catalyst dosage of 0.8 g（mass ratio of 4.25% in relation to phenol）.In the meantime,post-treatment with the addition of adequate water helps to increase the yield of the product and improve operability as well.