三光气法双酚芴型聚碳酸酯的合成  

Synthesis of BHPF-PC with Triphosgene

作　　者：鄂永胜[1] 鄢景森[1] 杨芳[1] 王泽青 E Yongsheng;YAN Jingsen;YANG Fang;WANG Zeqing(School of Biological and Chemical Engineering,Liaoning Institute of Science and Technology,Benxi,Liaoning 117004,China)

机构地区：[1]辽宁科技学院生物医药与化学工程学院,辽宁本溪117004

出　　处：《塑料》2022年第3期83-87,共5页Plastics

基　　金：辽宁省自然科学基金(20180550114)。

摘　　要：以三光气和双酚芴为原料,采用界面缩聚法合成双酚芴型聚碳酸酯,得到反应的最佳条件为三光气和双酚芴的摩尔比为1.3:3,催化剂三乙胺的含量为双酚芴含量的3.8%,反应温度为40℃,双酚芴和氢氧化钠的摩尔比为3:8,氢氧化钠的质量浓度为8%,三光气的二氯甲烷溶液浓度为0.195 mol/L,三光气的二氯甲烷溶液滴加时间≥40 min,总反应时间为100 min,快速搅拌,以热丙酮洗涤的方式进行后处理。采用红外吸收光谱分析产品结构,用乌氏黏度计测量样品的特性黏度,并计算出样品的黏均分子量为26000,差示扫描量热法检测出产物的玻璃化转变温度为232℃,这表明,新方法合成的双酚芴型聚碳酸酯具有良好的耐热性能。Using triphosgene and 9,9-bis(4-hydroxyphenyl)fluorene(BHPF)as raw materials,BHPF-PC was synthesized by interfacial polycondensation.The optimal conditions for the reaction were obtained.The molar ratio of triphosgene and BHPF was 1.3:3,the amount of catalyst(triethylamine)was 3.8%of the amount of BHPF,the reaction temperature was 40℃,the molar ratio of BHPF and sodium hydroxide was 3:8,the concentration of sodium hydroxide was 8%,the concentration of the dichloromethane solution of triphosgene was 0.195 mol/L,the dropping time of the dichloromethane solution of triphosgene was not less than 40 min,the total reaction time was 100 min,the stirring speed was fast and the post-treatment method was to wash with hot acetone.The structure of the product was verified by infrared absorption spectroscopy.The intrinsic viscosity of the sample was measured by ubbelohde viscometer and the viscosity average molecular weight of the sample was calculated to be 26000.The glass transition temperature of the product was detected to be 232℃by differential scanning calorimetry.This showed that the BHPF-PC synthesized by the new method had good heat resistance.

关 键 词：三光气 双酚芴 界面缩聚法 双酚芴型聚碳酸酯 合成 

分 类 号：TQ323.41[化学工程—合成树脂塑料工业]