| 松香基季铵盐为模板剂有序超微孔二氧化硅的合成 |
| Synthesis of Ordered Supermicroporous Silica Using Rosin-Based Quaternary Ammonium Salt |
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| 摘要: 以松香基季铵盐(脱氢枞基三甲基溴化铵,标记为DTAB)为模板剂、正硅酸乙酯为硅源、氨水为碱性介质成功合成出具有纳米片状形貌的六方有序超微孔二氧化硅材料。采用X射线衍射、N2吸附-脱附、透射电镜、扫描电镜等手段对样品进行表征,结果表明,体系中模板剂添加量、硅源添加量、碱性介质添加量、晶化温度、搅拌时间对前驱体的有序度有着较大的影响。当物质的量之比为nSiO2:nDTAB:nNH3:nH2O=1.0:0.1:11.3:924.0,晶化温度为373 K,搅拌时间为24 h,所得样品有序度最高。经煅烧后样品具有较大的比表面积(1 024 m2·g-1)和孔容(0.56 cm3·g-1),以及狭窄的孔径分布(集中于1.80 nm)。 |
| 关键词: 松香基季铵盐 有序超微孔 二氧化硅 |
| 基金项目: 教育部博士学科点专项科研基金课题(No.20133603120002)资助项目。 |
| Abstract: Ordered hexagonal supermicroporous silica with nanosheet morphology was successfully synthesized using rosin-based quaternary ammonium salt (dehydroabietyltrimethyl ammonium bromine, short for DTAB) as template agent, tetraethyl orthosilicate as silicate source, and ammonia as alkaline medium. XRD, N2 adsorption-desorption, TEM, and SEM were used to characterize the samples. The results indicated that the dosage amount of template agent, silicate source, alkaline medium, crystallization temperature and stirring time had great effects on the regularity of the pore structure. When the mole ratio of nSiO2:nDTAB:nNH3:nH2O was 1.0:0.1:11.3:924.0; crystallization temperature was 373 K; stirring time was 24 h, the sample got the hightest regularity. After the calcination, the synthesized material possessed large surface area (1 024 m2·g-1), high pore volume (0.56 cm3·g-1) and narrow pore size distribution (centered at about 1.80 nm). |
| Keywords: rosin-based quaternary ammonium salt supermicroporous silica |
| 投稿时间：2014-11-05 修订日期：2015-01-12 |
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| 王鹏,陈尚钘,黄敏,赵振东,王宗德,范国荣.松香基季铵盐为模板剂有序超微孔二氧化硅的合成[J].无机化学学报,2015,31(4):767-773. |
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