S Zorb吸附剂Rietveld物相定量方法研究

S Zorb技术是生产低硫清洁汽油的核心技术之一，在装置工业运行过程中发现吸附剂失活快、剂耗高等问题。为了研究吸附剂失活原因，并为国产剂的开发提供支持，利用X射线衍射（XRD）表征S Zorb工业装置中吸附剂的新鲜剂、待生剂和再生剂的晶体结构，探讨吸附剂物相变化规律，结果表明非活性锌类尖晶石的生成是导致吸附剂失活的主要因素。针对不同剂型的S Zorb吸附剂分别建立了Rietveld相定量方法，表征不同形态吸附剂晶相和非晶相物质的质量分数，并利用XRF方法表征吸附剂化学组成，进一步验证了Rietveld相定量法的准确性，利用²⁹Si NMR表征吸附剂中Si元素的化学环境，验证Rietveld相定量法对无定型SiO₂定量结果的准确性。Rietveld相定量法可广泛应用于S Zorb工业装置运行情况监控以及新剂的研究开发。

Study of Rietveld Quantitative Phase Analysis of S Zorb Sorbent

The S Zorb technology is a main technology for production of low-sulfur gasoline.During the plants operation,it was found that the sorbent was deactivation and consumption quickly.In order to study the deactivation reason,and to provide support for development of homemade sorbent,the crystal structures of S Zorb fresh,spent and regenerated sorbents were characterized by X-ray diffraction analysis(XRD).The law of phase transformation of sorbent was discussed.The deactivation of sorbent was mainly attributed to the present of non-active zinc-type spinel.The Rietveld quantitative phase analysis(RPA) method was established for S Zorb fresh,spent and regenerated sorbents,respectively,which could be used to determine the amount ratio of crystalline to amorphous phases in each sorbent.The chemical composition of sorbent was characterized by X-ray fluorescence analysis(XRF) to verify the accuracy of RPA.The amount of amorphous SiO2 was further determined by 29Si NMR analysis.The results obtained by XRD,XRF and 29Si NMR were found to complement each other well.Obviously,the RPA method can be widely used in online monitoring of industrial equipment and S Zorb sorbent development.