应用化学 ›› 2019, Vol. 36 ›› Issue (1): 51-57.DOI: 10.11944/j.issn.1000-0518.2019.01.180069

• 研究论文 • 上一篇    下一篇

以短链季铵盐/脂肪酸盐为模板合成超微孔二氧化硅

王仁亮,朱延美(),冀海伟   

  1. 泰山医学院化学与制药工程学院 山东 泰安 271016
  • 收稿日期:2018-03-13 接受日期:2018-06-07 出版日期:2019-01-01 发布日期:2019-01-04
  • 通讯作者: 朱延美
  • 基金资助:
    胶体与界面化学教育部重点实验室(山东大学)开放课题(201407)泰山医学院高层次课题培育计划(2015GCC19)山东省高等学校科技计划项目( J17KB072)资助

Synthesis of Ordered Supermicroporous Silica Using Short-Chain Quaternary Ammonium/Fatty Acid Salts as Template

WANG Renliang,ZHU Yanmei(),JI Haiwei   

  1. School of Chemistry and Pharmaceutical Engineering,Taishan Medical University,Taian,Shangdong 271016,China
  • Received:2018-03-13 Accepted:2018-06-07 Published:2019-01-01 Online:2019-01-04
  • Contact: ZHU Yanmei
  • Supported by:
    Supported by the Foundation of Key Laboratory of Colloid and Interface Chemistry(Shandong University), Ministry of Education(No.201407), Foundation for High-Level Project Development(No.2015GCC19), Science and Technology Research Program for Colleges and Universities(No.J17KB072)

摘要:

超微孔材料具有1~2 nm的孔径,在分离、催化应用中有望展现出择形催化的能力。 寻找经济、简便的合成超微孔材料的表面活性剂体系是一项有意义的工作。 本研究以短链季铵盐(十烷基三甲基溴化铵,记为C10TAB)和不同链长脂肪酸酸盐混合胶束为模板剂,硅酸钠为硅源,成功制备出高度有序超微孔SiO2。 通过小角X射线衍射、N2吸附-脱附、傅里叶变换红外光谱、扫描电子显微镜(SEM)和透射电子显微镜(TEM)等技术手段对产品的结构和性能进行了表征。 结果表明,合成体系中脂肪酸盐碳链长、加入量、晶化温度等对产物孔道有序性有很大影响。 当选择正辛酸钠(SO)为助表面活性剂,当n(C10TAB):n(Na2SiO3):n(SO):n(H2O)=1:1.5:0.3:800,晶化温度为80 ℃时,可以得到高度有序超微孔SiO2。 煅烧后样品比表面积为1300 m2/g,孔体积0.49 cm3/g,孔径分布在1.90 nm。

关键词: 超微孔二氧化硅, 短链季铵盐, 脂肪酸盐, 胶束, 混合表面活性剂

Abstract:

Supermicroporous materials possess pore size of 1~2 nm. They are expected to exhibit size- and shape-based separation/catalytic applications, which plays important role in modern industry. It is challenging to find an economic/simple surfactant system for the synthesis of supermicroporous materials. In this work, supermicroporous silica was synthesized using short-chain quaternary ammonium salt(decyltrimethyl ammonium bromide, denoted C10TAB) surfactant system mixed with fatty acid salts as the templating agents. The samples were characterized by small-angle X-ray diffraction(XRD), N2 adsorption-desorption, Fourier transform infrared spectroscopy(FTIR), scanning electron microscopy(SEM) and transmission electron microscopy(TEM). The results indicate that the length of alkyl chain in co-surfactant, the dosage amount, crystallization temperature have great effects on the regularity of the pore structure. We can obtain highly ordered supermicroporous silica when using sodium octanoate(denoted SO) as co-surfactant in the molar ratio of n(C10TAB):n(Na2SiO3):n(SO):n(H2O)=1:1.5:0.3:800, at the crystallization temperature of 80 ℃. The calcinated materials possess surface area 1300 m2/g and pore volume 0.49 cm3/g with a pore size distribution centered at about 1.90 nm.

Key words: supermicroporous silcia, short-chain quaternary ammonium salt, fatty acid salts, micellar, mixed surfactants system