含呋喃基双酚-双(4-羟基-3,5-二甲基苯基)呋喃甲烷的合成与表征

摘要

Bis ( 4-hydroxy-3,5-di-methylphenyl ) -furylmethane was synthesized by the condensation reaction using 2,6-xylenol and furfural as starting materials, sodium hydroxide as catalyst. The influence of various factors on this reaction was investigated. Orthogonal experiment was designed by selection of such major factors, as reaction temperature, catalyst dosage and reaction time. The optimum reaction conditions were determined as follows: 2.2∶ 1 of n(2,6-xylenol)/n(furfural), 1∶0.11 of n(2,6-xylenol)/n(sodium hydroxide), reaction temperature 65 ℃ and reaction time 5 h. Under the optimal conditions, the product yield could reach 61.7％. The structure of the product with purity of 99.52％ and melting point of 151.1 ℃ were confirmed by FTIR, 1H NMR and MS.%以2,6-二甲基苯酚和糠醛为原料,氢氧化钠为催化剂,经缩合反应合成了双(4羟基-3,5-二甲基苯基)呋喃甲烷.研究了各因素对反应收率的影响规律,选择反应温度、催化剂用量和反应时间为主要影响因素进行了正交实验.实验得出优化后反应条件为:n(2,6-二甲基苯酚):n(糠醛)=2.2∶1,n(2,6-二甲基苯酚):n(氢氧化钠)=1∶0.11,反应温度为65℃,反应时间为5h.在较优条件下进行实验,所得产物收率为61.7%.采用FTIR、1HNMR和MS表征确定了产物结构,并测得其熔点为151.1℃,纯度为99.52%.