以MgCl2·6H2O、AlCl3·6H2O、Na2CO3为原料,采用乙二醇—变频微波—水热法制备了优质镁铝水滑石。样品用XRD、SEM、TEM、IR、TG-DAT、N2吸附—解吸进行了物相、粒度、晶体形貌结构、红外分析、热分析和比表面分析。考察了传统水热法、变频微波—水热法、乙二醇—水热法、乙二醇—变频微波—水热法四种工艺对水滑石晶形、结构、分散性、规整性的影响。实验发现,在水热反应体系中加入φ=10%的乙二醇,调节变频微波炉反应温度为120℃,反应时间为5 h时可获得晶形好、板层结构显著、规整性好、分散性好的优质镁铝水滑石,透射电镜示粒子直径约在200 nm。
A regular nanocrystalline supramolecular Mg-Al hydrotalcite was prepared via glycol-frequency microwave-hydrothermal using MgCl2·6H2O,AlCl3·6H2O,Na2CO3 as raw material as precipitator.Hydrotalcite samples were characterized by X-ray diffraction(XRD),scan electron microscope(SEM),transmission electron microscope(TEM),IR,thermal analysis(TG-DTA),and BET-N2 surface area measurements.The images of SEM and TEM showed that the hydrotalcite exhibited as a homogeneous and hexagonal sheet.The XRD result indicated that the hydrotalcite was well crystallized.The influences of tradition hydrothermal,frequency microwave-hydrothermal and glycol-frequency microwave-hydrothermal on the sample character were investigated.A Mg-Al hydrotalcite with well-defined shape,obvious intercalated structure,well regular quality and well-dispersing capability was obtained when glycol volume ratio was 10% at 120 ℃ for 5 h.