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：刘洁翔[1] 张永清[1] 张晓光[2] 王建龙[1] 赵凌峰[1] 杨津[1] 王瑞[1] 

机构地区：[1]河北工业大学化工学院,天津300130 [2]南开大学化学学院,天津300071

出　　处：《无机化学学报》2014年第4期837-844,共8页Chinese Journal of Inorganic Chemistry

基　　金：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

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）和磺丁基醚串．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。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 pH value 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 DBS improved distinctly in the interlayer due to the strong supra-molecular interaction existed between anions and hostlayer of LHS.

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 磺丁基醚够-环糊精 热稳定性 

分 类 号：O641.813[理学—物理化学] O641.241[理学—化学]