低分子质量聚四氢呋喃二苯甲酸酯的合成及其应用  

Synthesis and application of low molecular weight polytetrahydrofuran dibenzoate

作　　者：李纲 张洋洋 钱俊峰[2] 何明阳[2] 陈群[2] LI Gang;ZHANG Yang-yung;QIAN Jun-feng;HE Ming-yang;CHEN Qun(l.Sinopec Great Wall Energy and Chemical(Ningxia)Co.,Ltd.,Yinchuan 750409,China;College of Petrochemical Engineering,Changzhou University,Changzhou 213164,China)

机构地区：[1]中石化长城能源化工(宁夏)有限公司,宁夏银川750409 [2]常州大学石油化工学院,江苏常州213164

出　　处：《现代化工》2020年第4期198-203,共6页Modern Chemical Industry

摘　　要：以TiO2/SiO2[n(TiO2)∶n(SiO2)=90∶10]为催化剂,催化合成了低分子质量聚四氢呋喃二苯甲酸酯(PTMGDB)。采用单因素法进行条件筛选,借助响应面分析法建立连续变量曲面模型,优化反应工艺并预测最佳反应工艺条件为:反应时间为4 h、反应温度为202℃、催化剂质量分数为0. 319%(占酸醇总质量)、n(苯甲酸)∶n(聚四氢呋喃)=2. 077∶1。预测的转化率为99. 96%,实验重复3次,酯化率高达99. 91%,相对误差为0. 05%,并通过FT-IR、GPC对产品结构进行表征。结果表明,该模型能成功预测酯化反应结果。加入10%PTMGDB增塑后,PVA水凝膜熔点从183. 5℃降低至116. 9℃,热稳定性提高;拉伸强度由77. 9 MPa降至38. 4 MPa;熔体流动速率由0. 005 g/min升至4. 28 g/min。因此,低分子质量PTMGDB可提高PVA热稳定性、力学性能及熔体流动性,可解决PVA难以热塑性加工的难题。Low molecular weight polytetrahydrofuran dibenzoate( PTMGDB) is synthesized by using TiO2/SiO2[n( TiO2) ∶n( SiO2) = 90 ∶10] as catalyst.The esterification process is optimized by adopting single factor method for condition screening and establishing a continuous variable surface model through response surface methodology. The predicted optimum reaction process conditions are determined as follows: reaction spends 4 h,reaction temperature is set at 202℃,catalyst dosage is 0. 319% of total mass of acid and alcohol,and n( benzoic acid) ∶ n( polytetrahydrofuran) =2. 077 ∶1.Conversion rate is predicted to be 99. 96%.The esterification rate is as high as 99. 91% with a relative error of0. 05% in three repeated experiments.It is indicated that the established model can successfully predict the results of this esterification reaction.What’s more,the structure of PTMGDB product is characterized by FT-IR and GPC. After being plasticized by adding 10% PTMGDB,the melting point of PVA hydrogel membrane is lowered from 183. 5℃ to 116. 9℃,its tensile strength declines from 77. 9 MPa to 38. 4 MPa,and its melt flow rate increases from 0. 005 g·min-1 to 4. 28 g·min-1.Therefore,it is verified that low molecular weight PTMGDB can help PVA improve thermal stability,mechanical properties and melt fluidity,thus overcoming the difficult in the thermoplastic processing of PVA.

关 键 词：低分子质量聚四氢呋喃二苯甲酸酯 酯化反应 响应面分析 PVA增塑 

分 类 号：TH3[机械工程—机械制造及自动化]