三酚基甲烷合成工艺的优化

Optimization of the Synthesis Process of Tri(4-hydroxyphenyl)methane

以苯酚、对羟基苯甲醛为原料,选用对甲苯磺酸和无水氯化铝为催化剂合成三酚基甲烷,利用红外光谱、液相色谱以及核磁共振等手段对产物进行表征,考察了反应温度、催化剂用量、原料配比及反应时间等工艺参数对产率的影响,随着反应温度的升高,产率逐渐下降;随着催化剂用量的增加,产率先增加后减少;随着原料配比的增加,产率逐渐增加趋于稳定。得出优化的工艺条件为:苯酚与对羟基苯甲醛的摩尔比为10∶1,对甲苯磺酸与对羟基苯甲醛质量比为1∶2,无水氯化铝与对羟基苯甲醛质量比为1∶6,反应时间为4h,温度为45℃,采用该工艺参数可使产率稳定在90%以上。纯化后的样品纯度高达99%以上。

The tri（4-hydroxyphenyl）methane was synthesized by using phenol and p-hydroxy benzaldehyde as feed stock,p-toluenesulfonic acid and aluminium chloride as catalyst.The chemical structure of tri（4-hydroxyphenyl）methane was characterized by Fourier-transform infrared（FTIR）spectrometer and 1 H NMR spectrometer.Four factors such as usage of catalyst,reaction temperature,material ratio and reaction time was studied in experiment,with the increasing of the reaction temperature,the yield increased;with the increasing of catalyst usage,the yield showed an earlier raised and later decreased;with the increasing of material ratio,the yield increased,and then trends toward constance.The result shows that the optional process is that n（phenol）/n（p-hydroxy benzaldehyde）is 10∶1,n（p-toluenesulfonic acid）/n（phydroxy benzaldehyde）is 1∶2,n（aluminium chloride）/n（p-hydroxy benzaldehyde）is 1∶6,reaction time is 4hand reaction temperature is 45℃.Under the processing parameter,the yield of product is up to 90%,the purity of the product is up to 99%.