镍锆钨杂多酸盐的制备、表征及性能测试

Synthesis and Characterization of Ni,Zr,W Heteropolyacid Salt

为了研究钨系杂多酸盐的超声催化性能,采用经典酸化法制备了1∶11系列镍、锆、钨三种金属的杂多酸盐.通过红外光谱、X射线衍射、紫外光谱对其结构进行了表征.利用热重/差热分析仪(TGA/DSC)对其热稳定性以及结晶水的数目进行了探究,并研究了该杂多酸盐催化剂的超声催化降解性能.以酸性墨绿配制模拟染料废水,考察了催化剂投加量、染料溶液初始浓度、反应溶液pH值和超声功率对超声催化降解染料废水的影响.研究结果表明:制备的镍锆钨杂多酸盐属于典型的Keggin型杂多酸盐,且具有良好的热稳定性.经过计算得出其化学表达式为Na_6[Ni(ZrW_(11)O_(39))]·20H_2O.在投加量为0.05g(即0.2g·L^(-1))、染料废水浓度为10mg·L^(-1)、pH值为4、超声频率为45kHz和功率为80%的条件下,染料废水的降解率达到95.65%.

To investigate the ultrasonic catalytic properties of tungsten heteropolyacid salts,NiZrW,a three metal salt of 1∶11 series heterolyacid salts,is synthesized via classic acidification method.And it is characterized by fourier transform infrared spectroscopy (FT-IR ),ultraviolet spectra (UV ),X-ray diffraction(XRD ).The thermogravimetric analysis/differential scanning calorimetry (TGA/DSC )is employed to validate the thermal stability and to calculate the number of crystallized water of the catalyst.The ultrasonic catalytic degradation performance of the heteropolyacid salt catalyst is also investigated.The characterization results state clearly that the catalyst possesses the typical Keggin structure,and is with good thermal stability and contained twenty three intramolecular crystallized water,thus the formula of the catalyst is Na6 [Ni(ZrW11 O39 )]·20H2 O.In the experiment,acidic blackish green is applied to exam the degradation ability of catalyst with ultrasonic waves,the effect of catalyst dosage,initial concentration,pH value and ultrasonic power on degradation rate is discussed.The results indicates that the optimum condition is observed at the catalyst dosage of 0.05 g(0.2 g·L-1 ),an initial concentration of 10 mg·L-1 ,an ultrasonic frequency of 45 kHz and an ultrasonic power of 80%.The degradation rate reaches up to 95.65% after 120 minutes irradiation.