异山梨醇与碳酸二甲酯两步法合成聚碳酸酯的工艺  

Two-step process for synthesizing polycarbonate from isosorbide and dimethyl carbonate

作　　者：陶国行 余锦涛[1] 魏永梅[1] 王涛[1] 田恒水[1] TAO Guohang;YU Jintao;WEI Yongmei;WANG Tao;TIAN Hengshui(School of Chemical Engineering,East China University of Science and Technology,Shanghai 200237,China)

机构地区：[1]华东理工大学化工学院

出　　处：《化工进展》2019年第10期4632-4638,共7页Chemical Industry and Engineering Progress

摘　　要：研究了以碳酸铷(Rb2CO3)和乙酰丙酮锂(LiAcac)为催化剂,异山梨醇(IS)和碳酸二甲酯(DMC)为原料合成聚碳酸酯(PC)的工艺过程。优化了酯交换反应催化剂用量、原料配比、缩聚反应催化剂用量、缩聚反应温度以及缩聚反应停留时间,并对酯交换产物和聚碳酸酯产品进行了红外光谱、核磁氢谱、核磁碳谱和热重分析,得到较优工艺条件为:Rb2CO3用量1×10^-3mol/molIS、原料配比n(DMC)/n(IS)=14、LiAcac用量2×10^-3mol/molIS、缩聚温度225℃、缩聚停留时间4h,所得的PC产品特性黏数可达36.55mL/g,数均分子量(Mn)为30659,重均分子量(Mw)为42551,Mw/Mn为1.39,色差为6.92,玻璃化转变温度(Tg)为155.6℃。Polycarbonate(PC) is synthesized from isosorbide(IS) and dimethyl carbonate(DMC)through transesterification and polycondensation reactions catalyzed by rubidium carbonate(Rb2CO3)and lithium acetylacetonate(LiAcac). The reaction conditions in both steps were fully optimized including the amount of the catalysts, ratio of the raw materials, polycondensation temperature, and the polycondensation residence time. Moreover, FTIR,1 H NMR,^13C NMR, and TGA technologies were used to characterize both transesterification and polycarbonate products. The optimum conditions were obtained as follows: the amount of Rb2CO3 1×10^-3 mol/molIS, the molar ratio of DMC/IS 14, the amount of LiAcac 2×10^-3 mol/molIS, polycondensation temperature of 225℃ and polycondensation retention time of 4 h. And the intrinsic viscosity, chromatic aberration, Tgof polymer PC could be up to 36.55 mL/g, 6.92, 155.6℃,respectively. The Mnof PC is 30659 and Mwis 42551 with Mw/Mnof 1.39, respectively.

关 键 词：催化剂 二元醇 聚合物 合成 优化 

分 类 号：TQ323.4[化学工程—合成树脂塑料工业]