固相法制备ZnO/改性半焦脱硫剂及其脱硫性能研究

Preparation of ZnO/modified semi-coke desulfurizer by solid state reaction and study on its performance of removing sulfide

采用固相法制备了Zn O/改性半焦脱硫剂,在固定床反应器上考察了负载比、活性组分质量分数、焙烧温度、焙烧时间和助剂质量分数对脱硫剂脱硫性能的影响,采用X射线衍射仪(XRD)、扫描电镜(SEM)、氮吸附技术对最优条件下制备的脱硫剂进行了表征。试验得到的Zn O/改性半焦脱硫剂的最佳制备条件为:负载比(Zn O与改性半焦质量比)5∶3,活性组分质量分数30%,焙烧温度600℃,焙烧时间2 h,助剂质量分数4%。固相法制备的脱硫剂结晶度好,脱硫剂脱硫前后比表面积、孔容、孔径变化较小,表明脱硫剂中载体改性半焦的孔隙结构未受到破坏,有利于脱硫剂的后期再生。

The ZnO/modified semi-coke desulfurizer is prepared by solid state reaction. The effects of the ratio of loading, mass fraction of active component and promoter, and calcination temperature and time on the performance of removing sulfide are investigated on the fixed bed reactor. The desulfurizer prepared under optimum conditions are characterized by X-ray diffraction（XRD） ,scanning e- lectron microscope（SEM） and N2 adsorption. The optimum conditions for preparing ZnO/modified semi-coke desulfurizer are obtained as follows： the ratio of loading （mass ratio of ZnO to modified semi-coke） is 5：3, the mass fraction of active component is 30%, the calcination temperature is 600 ~C, the calcinations time is 2 h, and the mass fraction of promoter is 4%. The crystallinity of desulfurizer prepared by solid-state method is improved, and the specific area, pore volume and pore size before and after sulfidation changes slightly which indicates that the pore structure of modified semi-coke has not been destroyed during sulfidation, which is favorable for the desulfurizer regeneration.