改进的卤化氰-酚法合成双酚A型氰酸酯

Synthesis of Bisphenol-A Dicyanate Ester by a Modified Cyanogens Halide-Phenol Method

采用“改进的卤化氰-酚法”法，通过加入助催化剂提高。活性氰中间体”的稳定性以实现高纯度、高收率双酚A型氰酸酯单体（BADCy）的合成。用傅立叶红外光谱法（FT-IR）表征了氰酸酯化反应程度、杂质对单体纯度的影响水平以及温度对氰酸酯化反应的影响等，用高效液相色谱法（HPLC）和示差扫描量热法（DSC）表征了产物的纯度及反应活性。结果表明“改进的卤化氰-酚”合成法有效地降低了溴化氰过量率和三乙胺过量率对氰酸酯化程度及杂质水平的影响，反应温度可以提高到0℃～10℃的范围内，反应时间也随之缩短．得到了高纯度（〉99％）和高收率（〉95％）的BADCy单体。

Bisphenol-A dicyanate ester （BADCy） was synthesized by use a modified cyanogens halide-phenol method, which the main idea was to add a co-catalyst into the synthetic system to improve the stability of the ‘active cyanogens ＇ intermediate and fulfill the high purity and high yield BADCy synthesize. The degree of cyanation, effectives of impurities and temperatures on the cyanate reactions were characterized by Fourier transform infrared spectroscopy （FT-IR）. High performance liquid chromatography （HPLC） and differential scanning calorimeter （DSC） was used to characterize the purity of synthesized monomer and its reactivity. The result shows that the effect of excess of cyanogens bromide on the degree of cyanation reaction and the excess of triethylamine on impurity contents has sufficiently lowed in the modified method. Temperatures of synthesis reaction can be elevated to 0 ℃-10 ℃. Thus the reaction time is shortened. High purity （〉99%） and high yield （〉95%） BADCy monomer has been obtained.