1,4-环己烷二甲醇型聚碳酸酯二元醇的合成与表征  

Synthesis and Characterization of 1,4-cyclohexane Dimethyl Alcohol Modified Polycarbonate Diol

作　　者：刘静月 侯洪波 李贤勇 曾宪光 蒲泽军 钟家春 LIU Jingyue;HOU Hongbo;LI Xianyong;ZENG Xianguang;PU Zejun;ZHONG Jiachun(School of Materials Science and Engineering,Sichuan University of Science&Engineering,Zigong 643000,China)

机构地区：[1]四川轻化工大学材料科学与工程学院,四川自贡643000

出　　处：《四川轻化工大学学报（自然科学版）》2021年第4期18-24,共7页Journal of Sichuan University of Science & Engineering(Natural Science Edition)

基　　金：四川省科技厅重点研发项目(2018GZ0434)。

摘　　要：以1,4-环己烷二甲醇(CHDM)、碳酸二乙酯(DEC)、1,4-丁二醇(BDO)和1,6-己二醇(HDO)为原料,以钛酸正丁酯(TBT)为催化剂,通过酯交换反应分别合成了聚1,4-环己基碳酸酯二醇(PCH⁃DL)、1,4-环己基-丁基碳酸酯二醇(PCHBDL)和聚1,4-环己基-己基碳酸酯二醇(PCHHDL)。通过傅里叶红外光谱(FT-IR)、核磁氢谱(1H-NMR)、热重(TG)、差示扫描量热(DSC)及羟值与分子量测定等方法对产物进行了表征。结果显示所合成的聚碳酸酯二元醇产物分子量分别为1063 g/mol、1376 g/mol、1553 g/mol,FT-IR结果表明产物结构具有碳酸酯基与羟基,为聚碳酸酯二元醇的典型结构,与1H-NMR所表明PCHDL、PCHBDL和PCHHDL的结构一致。聚碳酸酯二元醇产物初始热分解温度大于200℃,玻璃化转变温度范围为-33.2℃~0℃。A series of novel polycarbonate diols(PCDLs)such as poly(1,4-cyclohexyl carbonate diol)(PCHDL),poly(1,4-cyclohexyl-butyl carbonate diol)(PCHBDL)and poly(1,4-cyclohexyl-hexyl carbonate diol)(PCHHDL),are synthesized via ester exchange reaction,using diethyl carbonate(DEC),1,4-cyclohexanedimethanol(CHDM)and 1,4-butanediol(BDO)or 1,6-hexanediol(HDO)as raw materials,with tetrabutyl titanate(TBT)as catalyst.The products are characterized by Fourier infrared spectroscopy(FT-IR),proton nuclear magnetic spectroscopy(1H-NMR),thermogravimentry(TG),differential scanning calorimetry(DSC)and determination of hydroxyl value and molecular weight.The results show that molecular weight of the synthesized PCDLs are 1063 g/mol,1376 g/mol and 1553 g/mol.FT-IR results suggest that the molecular structure of PCDLs has the carbonate base and hydroxyl,which is the typical structure of polycarbonate diol,and consistent with the structures of PCHDL,PCHBDL and PCHHDL characterized by 1H-NMR.The initial thermal decomposition temperature of the polycarbonate diol product is higher than 200℃,and the glass transition temperature ranges from-33.2℃to 0℃.

关 键 词：聚碳酸酯二元醇 1 4-环己烷二甲醇 碳酸二乙酯 合成 

分 类 号：TQ323.41[化学工程—合成树脂塑料工业]