| 模板剂缓释法合成分子筛大单晶 |
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| 引用本文： | 陈飞剑,林清芳,高子豪,沈福志,梁丽丽,杨贞,杜红宾. 模板剂缓释法合成分子筛大单晶[J]. 无机化学学报, 2016, 32(7): 1283-1292 |
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| 作者姓名： | 陈飞剑 林清芳 高子豪 沈福志 梁丽丽 杨贞 杜红宾 |
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| 作者单位： | 南京大学化学化工学院配位化学国家重点实验室, 南京 210023;蚌埠医学院化学教研室, 蚌埠 233030,蚌埠医学院化学教研室, 蚌埠 233030,南京大学化学化工学院配位化学国家重点实验室, 南京 210023,蚌埠医学院化学教研室, 蚌埠 233030,蚌埠医学院化学教研室, 蚌埠 233030,南京大学化学化工学院配位化学国家重点实验室, 南京 210023,南京大学化学化工学院配位化学国家重点实验室, 南京 210023 |
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| 基金项目： | 国家自然科学基金（No.21071075）、配位化学国家重点实验室开放课题计划（No.SKLCC201507）、安徽高校自然科学研究项目（No.KJ2016A462，KJ2016A463）和蚌埠医学院自然科学基金项目（No.BYKC1401ZD，BYKY1433）资助。 |
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| 摘 要： | 在分子筛的合成中，通过使用四咪唑基取代的硼类化合物（四咪唑硼钠）作为模板剂，在溶剂热条件下，成功得到了磷酸铝盐分子筛AlPO4-11的大单晶。电喷雾质谱、19F和11B NMR等研究结果表明，在溶剂热条件下四咪唑硼钠起到了缓释剂的作用，其自身经历缓慢分解，持续释放低浓度咪唑分子的过程。由其释放出来的咪唑分子起到事实上的模板作用。因其浓度较低，限制了分子筛结晶过程中晶核形成的数量，从而易于导向分子筛大单晶的生成。通过引入不同种类的四取代硼类化合物作为模板剂，这种分子筛大单晶的合成策略可潜在应用于其它分子筛材料。
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| 关 键 词： | 模板剂 分子筛 单晶 合成 |
| 收稿时间： | 2016-03-15 |
| 修稿时间： | 2016-05-23 |
Synthesis of Large Zeolite Crystals Through Slow Release of Structure-Directing Agents |
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| CHEN Fei-Jian,LIN Qing-Fang,GAO Zi-Hao,SHEN Fu-Zhi,LIANG Li-Li,YANG Zhen and DU Hong-Bin. Synthesis of Large Zeolite Crystals Through Slow Release of Structure-Directing Agents[J]. Chinese Journal of Inorganic Chemistry, 2016, 32(7): 1283-1292 |
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| Authors: | CHEN Fei-Jian LIN Qing-Fang GAO Zi-Hao SHEN Fu-Zhi LIANG Li-Li YANG Zhen DU Hong-Bin |
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| Affiliation: | State Key Laboratory of Coordination Chemistry, School of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210023, China;Department of Chemistry, Bengbu Medical College, Bengbu, Anhui 233030, China,Department of Chemistry, Bengbu Medical College, Bengbu, Anhui 233030, China,State Key Laboratory of Coordination Chemistry, School of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210023, China,Department of Chemistry, Bengbu Medical College, Bengbu, Anhui 233030, China,Department of Chemistry, Bengbu Medical College, Bengbu, Anhui 233030, China,State Key Laboratory of Coordination Chemistry, School of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210023, China and State Key Laboratory of Coordination Chemistry, School of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210023, China |
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| Abstract: | By using imidazole-substituted quaternary boron compound NaB(Im)4 (Im=imidazole) as a structure directing agent (SDA) in the zeolite synthesis, we successfully obtained single crystals of aluminophosphate AlPO4-11 under solvothermal conditions. Electrospray ionization mass spectrometry, 19F and 11B NMR studies showed that these quaternary boron compounds acted as SDA buffers, undergoing the decomposition process to slowly release a low concentration of imidazole molecules under solvothermal conditions. The latter served as SDAs to form a limited number of zeolite nuclei, thus leading to the growth into large single crystals. Under similar conditions, the direct use of the corresponding free imidazole molecules in the synthesis produced only fine powders. This approach could be potentially applied to synthesize large crystals of other zeolites, given the availability of various quaternary boron compounds. |
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| Keywords: | structure-directing agents zeolite single crystal synthesis |
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