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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。
Abstract
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 of 0.05% 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
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PVA增塑
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响应面分析
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酯化反应
Key words
low molecular weight PTMGDB
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plasticization of PVA
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response surface methodology
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esterification reaction
Author summay
李纲(1984-),男,工学学士,工程师,研究方向为BDO与PTMEG的生产及应用,ligang.nxnh@sinopec.com
低分子质量聚四氢呋喃二苯甲酸酯的合成及其应用[J].
现代化工, 2020, 40(4): 198-203 DOI:10.16606/j.cnki.issn0253-4320.2020.04.042