以ZnSO4、FeSO4为原料,采用共沉淀和氧化的两步法合成了ZnFe^Ⅲ二元类水滑石化合物,详细探讨了原料配比、PH及氧化处理条件等因素对合成产物物相的影响。借助XRD,FTIR,N2吸附等手段对合成物物化性能进行表征。研究结果表明:以Zn(NO3)2、Fe(NO3)3为原料,改变合成条件只能得到碱式碳酸锌或碱式硝酸锌;而以FeSO4、FeSO4为原料,采用共沉淀和氧化的两步法可得到晶相单一、结晶度良好的ZnFe^Ⅲ HTLCS。两步法制备ZnFe^Ⅲ类水滑石的最适宜的条件为:n(Zn^2+)/n(Fe^2+)=2.0~3.0,PH=6.0~7.0,氧化温度为25℃,该条件下合成的ZnFe^Ⅲ HTLCS有较高的热稳定性,热分解温度为600℃;有较窄的粒径分布,中值粒径为1.24μm,平均粒径为1.28/zm;吸附等温线类型为Ⅱ型,比表面积为23.08m^2/g。
ZnFe^Ⅲ-hydrotalcite-like-compounds (ZnFe^Ⅲ HTLcs) were synthesized from ZnSO4 and FeSO4 by two-step method, i.e. co-precipitation and subsequent oxidation by H2 02. The influence of the parameters such as ratio of materials, pH value and the oxidation condition, was discussed. Characteriza- tion of samples was carried out by XRD, FTIR, and N2-adsorption. The results show that basic zinc carbonate or alkaline zinc nitrate was obtained from Zn(NO3 )2 and Fe(NO3)3 by changing the synthesis conditions. However, a single crystalline phase ZnFe^Ⅲ HTLcs with high erystallinity was obtained from ZnSO4 and FeSO4 by the two-step method. The optimized condition for the preparation of ZnFe^Ⅲ HTLcs by two-step method was, n(Zn^2+ )/n(Fe^2+ ) =2.0-3.0, pH=6.0-7.0, and the oxidation temperature 25 ℃. The prepared ZnFe111 HTLcs showed excellent thermal stability and narrow particle size distribution. The thermal decomposition temperature was 600℃. Median particle size was 1.24 μm and average particle size was 1.28 μm. The adsorption isotherms of the ZnFe^Ⅲ HTLcs belonged to Ⅱ-type and the specific surface area was 23.08 m^2/g.