氢氧化物盐插层材料的制备和表征
Preparation and Characterization of Intercalation Materials with Layered Hydroxide Salts (LHS)
作者单位E-mail
刘洁翔 河北工业大学化工学院, 天津 300130 jxliu@hebut.edu.cn 
张永清 河北工业大学化工学院, 天津 300130  
张晓光 南开大学化学学院, 天津 300071 xgzhang@nankai.edu.cn 
王建龙 河北工业大学化工学院, 天津 300130  
赵凌峰 河北工业大学化工学院, 天津 300130  
杨津 河北工业大学化工学院, 天津 300130  
王瑞 河北工业大学化工学院, 天津 300130  
摘要: 以层状氢氧化锌硝酸盐(Zn-LHS)和氢氧化镍锌硝酸盐(NiZn-LHS)为主体,采用共沉淀和离子交换法制备十二烷基苯磺酸根离子(DBS)和磺丁基醚-β-环糊精(SBE-β-CD)插层氢氧化物盐(Zn-LHS-DBS和NiZn-LHS-SBE-β-CD),系统考察客体阴离子浓度和pH值等因素对插层材料超分子结构的影响,并用XRD、FT-IR、TG-DTA和SEM对其结构、热稳定性和形貌等进行表征。结果表明,采用共沉淀法在DBS浓度为0.19~0.38mol·L-1,pH=6.0~7.0,水热温度60~100℃条件下合成晶型单一且结构完整Zn-LHS-DBS;采用离子交换法可合成结构完整NiZn-LHS-SBE-β-CD;无论离子交换还是共沉淀法都不能合成单一晶型Zn-LHS-SBE-β-CD,这可能与SBE-β-CD分子结构以及Zn-LHS水热稳定性差有关。此外,由于氢氧化物盐层板和客体间存在超分子作用而导致DBS和SBE-β-CD在层间具有较高热稳定性。
关键词: 氢氧化锌硝酸盐  氢氧化镍锌硝酸盐  十二烷基苯磺酸钠  磺丁基醚-β-环糊精  热稳定性
基金项目: 河北省自然科学基金(No.B2011202118);山东大学胶体与界面化学教育部重点实验室开放课题(No.201202);河北省高等学校科学技术研究项目(No.QN20131050)、“大学生创新创业训练计划”国家级项目(No.201310080018)资助项目。
Abstract: Intercalation of dodecyl benzene sulphonate (DBS) and sulfobutyl ether β-cyclodextrin (SBE-β-CD) into layered zinc hydroxide nitrate (Zn-LHS) and nickel/zinc hydroxide nitrate (NiZn-LHS) was synthesized by coprecipitation and ion-exchanged methods. The effect of anion concentration and pHvalue on preparation was systematically investigated and compared. The products were characterized by X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), and thermogravimetry and differential thermal analysis (TG-DTA), and scanning electron microscope (SEM). The results showed that Zn-LHS-DBS with pure phase and good crystallinity was obtained at DBS concentration of 0.19~0.38 mol·L-1, pH=6.0~7.0, temperature of hydrothermal treatment of 60~100 ℃ by coprecipitation method. The NiZn-LHS-SBE-β-CD with good structure was prepared by ion-exchanged method. Zn-LHS-SBE-β-CD with pure phase was not successfully prepared by both coprecipitation and ion-exchanged method due to the particular structure of SBE-β-CD and poor hydrothermal stability of Zn-LHS. Furthermore, TG-DTA data indicated that stability of SBE-β-CD and DBSimproved distinctly in the interlayer due to the strong supra-molecular interaction existed between anions and hostlayer of LHS.
Keywords: zinc hydroxide nitrate  nickel/zinc hydroxide nitrate  dodecyl benzene sulphonate  sulfobutyl ether β-cyclodextrin  thermostability
投稿时间:2013-09-15 修订日期:2013-11-18
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刘洁翔,张永清,张晓光,王建龙,赵凌峰,杨津,王瑞.氢氧化物盐插层材料的制备和表征[J].无机化学学报,2014,30(4):837-844.
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