超声辅助H_(2)O_(2)脱除炼焦煤中有机硫的方法及机理研究

Study on Method and Mechanism of Ultrasonic-assisted H_(2)O_(2) Removal of Organic Sulfur from Coking Coal

采用超声辅助过氧化氢(H_(2)O_(2))与冰乙酸(HAc)形成的氧化体系对新阳(XY)高有机硫焦煤进行脱硫实验。通过控制变量法,研究了固液比、反应时间、反应温度与煤样粒度等单因素对煤样脱硫效果的影响,设计了4因素3水平的正交实验,进一步确定各因素在煤样脱硫中最优水平组合。结果表明最佳脱硫条件为:反应温度50℃、反应时间1 h、固液比1 g(煤)∶1 mL(H_(2)O_(2))、煤样粒径小于1 mm,最佳脱硫条件下脱硫率为10.41%。利用傅立叶变换红外光谱仪(FTIR)和X射线电子能谱仪(XPS)对脱硫前后煤样的官能团结构及硫形态的变化进行测试。结果表明:氧化脱硫后煤样中含氧官能团和脂肪结构的含量均出现不同程度的下降,煤中低价态的硫醇/醚向高价态的(亚)砜类转化,最后可通过水洗达到脱硫目的。

The oxidation system formed by ultrasonic assisted hydrogen peroxide(H 2O 2)and glacial acetic acid(HAc)was used to desulfurization experiment of Xinyang(XY)high organic sulfur coking coal.The effects of single factors such as the solid-liquid ratio,reaction time,reaction temperature and coal sample particle size on the desulfurization were studied by controlling variable method.The orthogonal experiment of 4 factors and 3 levels was designed.The optimal level combination of various factors in coal desulfurization was determined.The experimental results show that the best desulfurization conditions are reaction temperature 50℃,reaction time 1 h,solid-liquid ratio 1 g(coal)∶1 mL(H_(2)O_(2)),and coal sample size less than 1 mm,under the optimal desulfurization conditions the desulfurization rate is 10.41%.The changes of functional group structure and sulfur morphology of coal samples before and after desulfurization were measured by Fourier transform infrared spectroscopy(FTIR)and X-ray electron spectroscopy(XPS).The results show that the oxygen-containing functional groups and fat structure in coal samples decrease to varying degrees after oxidative desulfurization.The low-valence mercaptan/ether in the coal are transformed into high-valence sulfoxide or sulfones.Finally,the desulfurization is achieved by washing coal with water.