A selective organosilica membrane for ethyl acetate dehydration by pervaporation
A selective organosilica membrane for ethyl acetate dehydration by pervaporation
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用于渗透蒸发乙酸乙酯脱水的选择性有机硅膜
DOI：
10.1002/app.50942
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发表时间：
2021-04
影响因子：
3
通讯作者：
Zhang Yan
中科院分区：
文献类型：
--
作者：
Raza Waseem;Jianhua Yang;Wang Jiaxuan;Saulat Hammad;Wang Lei;Lu Jingming;Zhang Yan
研究了有机硅双(三乙氧基硅基)乙烷(BTESE)膜对乙酸乙酯(EA)二元和三元混合物的渗透汽化脱水。通过改变聚合物溶胶中BTESE的浓度(分别为0.5、2.5和5wt%BTESE)，在大孔载体上制备了三种BTESE膜(M1、M2和M3)。用差示扫描量热法、扫描电子显微镜、傅立叶变换红外光谱、X射线衍射仪、接触角、原子力显微镜和渗透汽化性能对膜进行了表征，讨论了聚合物溶胶中BTESE含量对有机硅膜的形成和脱水性能的影响。结果表明，当BTESE的负载量为5wt%时，膜对EA/H2O混合体系的脱水具有较高的选择性。在合成的膜中，M3的通量为0.84kg.m ± 0.05kg.m −2.h−1，选择性为>；在60℃下，EA/H2O(98/2wt%)的渗透汽化脱水时间为10,000。EA/H2O(95/5wt%)渗透汽化脱水的时间过程证实了BTESE膜在所研究的120 h内是稳定的。此外，该膜对乙酸乙酯/乙醇/水和乙酸丙酯/异丙醇/水(90/2/8wt%)三元混合物(90/2/8wt%)的分离选择性分别大于10,000，其组成与工业酯化过程中精馏塔的顶产物相似。本研究中BTESE膜的最佳分离性能和良好的酸稳定性表明，未稀释的溶胶涂层和闪速烧成的简单合成方案将为实际的膜应用提供一条经济、快速、高效的合成路线。
Organosilica bis(triethoxysilyl) ethane (BTESE) membranes were explored for pervaporation dehydration of binary and ternary mixtures of ethyl acetate (EA) by undiluted sol coating combined with flash firing. Three BTESE membranes (M1, M2, and M3) were fabricated on macroporous supports by varying BTESE concentrations (0.5, 2.5, and 5 wt% BTESE, respectively) in polymer sols. The membranes were characterized by DLS, SEM, FTIR, XRD, contact angle, AFM, and pervaporation performance to discuss the effect of the BTESE contents in the polymer sol on the formation and dehydration performance of resulting organosilica membranes. It was found that 5 wt% loading of BTESE led to a highly selective membrane for dehydration of EA/H2O mixture. Among the synthesized membranes, M3 delivered flux of 0.84 ± 0.05 kg.m−2.h−1with a selectivity of >10,000 for EA/H2O mixture (98/2 wt%) at 60°C. The time course of pervaporation dehydration for the EA/H2O mixture (95/5 wt%) confirms the stability of BTESE membrane in the investigated time period of 120 h. Further, the membrane exhibited excellent selectivity larger than 10,000 for separation of ternary mixtures (90/2/8 wt%) of ethyl acetate/ethanol/water and n‐propyl acetate/isopropanol/water respectively, the composition of which is similar to the top product of the distillation column used in the industrial esterification process. The best separation performance and excellent acid stability of BTESE membranes in this study suggest that the simple synthesis protocol of undiluted sol coating and flash firing will provide a cost‐effective, quick, and efficient synthesis route for practical membrane based applications.
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