氧化锆湿凝胶中乙酰丙酮配体的脱除机理及气凝胶复合材料的制备  

Mechanism of the Removal of Acetylacetone Ligands in Zirconia Wet Gel and Fabrication of Zirconia Aerogel Composites†

作　　者：李占峰 刘本学 刘晓婵 王新强[2] 张晶 于诗摩 赵新富 张新恩 伊希斌 LI Zhanfeng;LIU Benxue;LIU Xiaochan;WANG Xinqiang;ZHANG Jing;YU Shimo;ZHAO Xinfu;ZHANG Xin’en;YI Xibin(Advanced Material Institute,Qilu University of Technology(Shandong Academy of Sciences),Jinan 250014,China;State Key Laboratory of Crystal Materials,Institute of Crystal Materials,Shandong University,Jinan 250100,China)

机构地区：[1]齐鲁工业大学(山东省科学院)新材料研究所,济南250014 [2]山东大学晶体材料国家重点实验室,晶体材料研究所,济南250100

出　　处：《高等学校化学学报》2021年第9期2904-2910,共7页Chemical Journal of Chinese Universities

基　　金：山东省自然科学基金(批准号:ZR2020QE037,ZR2019MEM034);齐鲁工业大学(山东省科学院)产学研协同创新基金(批准号:2020-CXY35)资助.

摘　　要：利用正硅酸四甲酯、正硅酸四乙酯、硼酸三乙酯浸泡聚乙酰丙酮合锆湿凝胶,通过红外光谱(IR)、元素分析(EA)、X射线光电子能谱(XPS)和色谱-质谱联用(GC-MS)等技术证实了有机硅(硼)烷浸泡湿凝胶可加速乙酰丙酮配体的脱除,并推断了相关反应机理.利用正硅酸四甲酯浸泡聚乙酰丙酮合锆湿凝胶显著强化了凝胶骨架,通过低成本干燥技术可以获得纳米多孔、高比表面积的ZrO2气凝胶.在石英纤维增强的ZrO2气凝胶复合材料中,纤维骨架进一步阻止了干燥收缩,微波干燥即可获得超轻质石英纤维/二氧化锆气凝胶复合材料(SFZA),稳态平板测试结果表明,其在1000℃下的导热系数最低可至0.042 W∙m^(−1)∙K^(−1),1200℃下导热系数最低可至0.063 W∙m^(−1)∙K^(−1).It was reported that the removal of acac ligands can be accelerated by soaking polyacetylacetonato-zirconium(PAZ)wet gel in organic silane(tetramethyl orthosilicate,tetraethyl orthosilicate)or organic borane(triethyl borate).Moreover,it was confirmed that soaking wet gel in siliane(borane)can accelerate the removal of acac ligands through infrared spectrum,elemental analysis,X-ray photoelectron spectroscopy,chromatography-mass spectrometry,etc.Meanwhile,the mechanism was be deduced.By soaking PAZ wet gel in organic silane,the gel skeleton was strengthened as well.Therefore,nanoporous ZrO2 aerogels with high specific surface area could be obtained by inexpensive drying techniques.In addition,to prepare the ultra-lightweight silica fiber/zirconia aerogel(SFZA),the ZrO2 aerogel matrix was also composite with ultrafine quartz fiber,which further prevents drying shrinkage.Based on the plate heat flow method the lowest thermal conductivity coefficient of the SFZA was 0.042 and 0.063 W∙m^(−1)∙K^(−1) at 1000 and 1200℃,respectively.

关 键 词：氧化锆气凝胶 复合材料 聚乙酰丙酮合锆 隔热材料 

分 类 号：O648[理学—物理化学] O614.41[理学—化学]