固相法制备半焦负载铁酸锌脱硫剂的脱硫行为

doi:10.16085/j.issn.1000-6613.2016-2192

摘要/Abstract

摘要： 以改性半焦为载体，通过固相法合成了铁酸锌脱硫剂，并在固定床上硫化温度500℃下考察了焙烧温度、焙烧时间以及铁酸锌的含量对脱硫剂的结构及脱硫性能的影响。实验结果表明最佳制备条件为铁酸锌含量为25%、焙烧温度为600℃、焙烧时间为2h，此时脱硫剂穿透时间和硫容最大分别为10.5h和8.58g/100g。采用X射线衍射（XRD）、氮吸附（BET）、X光电子能谱（XPS）、扫描电子显微镜（SEM）等方法对最佳制备条件的脱硫剂的新鲜样和硫化样的物相组成、孔结构、表面元素、外观形貌等进行表征。结果显示改性半焦能够提高铁酸锌脱硫剂的比表面积和孔隙度，并且制备的铁酸锌粒径较小，避免了团聚现象。另外SEM结果显示铁酸锌呈球形颗粒均匀地分散在半焦表面，可以为硫化反应提供更大的反应面积和促进质量传递。

关键词: 固定床, 固相法, 改性半焦, 铁酸锌, 硫化氢

Abstract: Modified semi-coke supported zinc ferrite sorbents were synthesized by mechanochemical method.The desulfurization ability of the sorbent was evaluated using a fixed-bed reactor at 500℃.The effects of calcination temperature,calcination time and zinc ferrite content of the sorbent on the structure and desulfurization performance were studied.The results showed that the optimum preparation conditions are as follows:25% active component,calcined for 2h at 600℃,and it's breakthrough time and sulfur capacity are 10.5h and 8.58(g S/100g sorbent),respectively.The fresh and used desulfurizers were characterized by X-ray diffraction (XRD),N₂ adsorption,scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy.The results indicated that the modified semi-coke can improve the specific surface area and porosity of the zinc ferrite desulfurizer,and the prepared zinc ferrite particle size is smaller to avoid agglomeration.In addition,the SEM results showed that the spherical particles of zinc ferrite are evenly distributed on the semi-coke surface,which can provide a larger reaction area and promote mass transfer for the sulfidation.

Key words: fixed-bed, mechanochemical method, modified semi-coke, zinc ferrite sorbent, hydrogen sulfide

中图分类号:

TQ02

苏子兵, 武蒙蒙, 贾磊, 张帅国, 米杰. 固相法制备半焦负载铁酸锌脱硫剂的脱硫行为[J]. 化工进展, 2017, 36(07): 2684-2690.

SU Zibing, WU Mengmeng, JIA Lei, ZHANG Shuaiguo, MI Jie. Preparation of zinc ferrite sorbent by mechanochemical method for the removal of H₂S from hot coal gas[J]. Chemical Industry and Engineering Progress, 2017, 36(07): 2684-2690.

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