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作 者:倪邦庆[1] 刘慧[1] 范明明[1] 张萍波[1] NI Bang-Qing LIU Hui FAN Ming-Ming ZHANG Ping-Bo(School of Chemical and Material Engineering, Jiangnan University, Key Laboratory of Food Colloids and Biotechnology, Ministry of Education, Wuxi, Jiangsu 214122, China)
机构地区:[1]江南大学化学与材料工程学院,食品胶体与生物技术教育部重点实验室,无锡214122
出 处:《无机化学学报》2017年第1期97-105,共9页Chinese Journal of Inorganic Chemistry
基 金:国家自然科学基金(No.21306063)资助项目
摘 要:采用一步共缩合-水热法合成酸性载体SO_4^(2-)/ZrO_2-SiO_2,化学法接枝酸性离子液体磺酸功能化咪唑硫酸氢盐([Ps-im]HSO4),构筑拥有Br觟nsted与Lewis双酸位的离子液体固载型催化剂SO_4^(2-)/ZrO_2-SiO_2-IL。采用X射线衍射、傅里叶红外、N2吸附-脱附、X射线光电子能谱、热重以及透射电镜对催化剂的结构进行表征,结果表明:锆原子和酸性结构SO42-被成功引入纯硅材料,所合成的载体具有一定酸性;离子液体成功固载于酸性介孔材料SO_4^(2-)/ZrO_2-SiO_2,且固载后的催化剂保持其介孔结构。以大豆油和甲醇的酯交换反应为探针,考察了SO_4^(2-)/ZrO_2-SiO_2-IL催化剂的催化性能。在反应温度为150℃、反应时间为4 h、催化剂量5%(w/w)、醇油物质的量之比为24∶1的反应条件下,生物柴油的收率超过92%,且回收利用5次后,生物柴油的收率仍达86%。The immobilized catalyst SO42-/ZrO2-SiO2-IL with double-acid active sites, namely Br?nsted and Lewis acid sites, was synthesized by immobilization of acid ionic liquid sulfonic acid functionalized imidazolium hydrogen sulfate([Ps-im]HSO4) onto the surface of the acidic mesoporous material SO42-/ZrO2-SiO2 which was prepared by a one-step co-condensation technique combined with hydrothermal treatment. The structure of the catalyst was characterized by XRD, FT-IR, N2 absorption-desorption measurement, XPS, thermogravimetric analysis and TEM. The results showed that zirconium and acid structure (SO42-) were incorporated into the framework of pure silicon, bringing a certain acidity; and it also demonstrated that the ionic liquid was successfully immobilized onto the acidic mesoporous materials SO42-/ZrO2-SiO2 and the structure of the catalyst remained intact. The activity of SO42-/ZrO2-SiO2-IL was investigated by the transesterification of soybean oil with methanol for biodiesel production as the probe reaction. The yield of biodiesel was more than 92% when the reaction was carried out under the following condition:reaction temperature, 150℃; reaction time, 4 h; amount of catalyst, 5%(w/w); methanol to soybean oil, 24:1. And the catalyst still yielded about 86% after five cycles.
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