NiWO_4/g-C_3N_4的制备及其在离子液体中氧化脱硫性能的研究

Preparation of NiWO4/g-C_3N_4 and its ultra-deep desulfurization properties in ionic liquid

采用水热法合成了NiWO_4纳米粒子,然后通过混合煅烧法成功地制备了负载型催化剂NiWO_4/g-C_3N_4。采用XRD、FT-IR、EDS、SEM、BET和XPS表征了NiWO_4/g-C_3N_4的形貌和结构特征。以NiWO_4/g-C_3N_4为催化剂,过氧化氢为氧化剂,1-丁基-3-甲基咪唑四氟硼酸盐离子液体([BMIM]BF4)为萃取剂。考察了催化剂的负载量,过氧化氢、离子液体和催化剂使用量,反应温度,反应时间,不同种类的含硫化合物对脱硫效果的影响。结果表明,在5 m L模拟油,0.2 m L过氧化氢,1.0 m L的[BMIM]BF4,0.03 g的NiWO_4/g-C_3N_4,反应温度为80℃,反应时间为140 min的最佳的反应条件下,脱硫率可以达到97.35%。实验表明,NiWO_4/g-C_3N_4具有很好的催化稳定性,催化剂重复使用五次后催化活性并没有明显地降低。

The NiW04nanoparticles were synthesized by hydrothermal method.The supported catalysts NiW04/g-C3N4were prepared by a simple mixing-calcination method.XRD,FT-IR,EDS,SEM,BET and XPS were used to characterize the morphology and structure of NiW04/g-C3N4.The prepared NiW04/g-C3N4was used as catalyst,hydrogen peroxide as oxidant,1-butyl-3-methylimidazolium tetrafluoroborate ionic liquid([BMIM]BF4)as extractant for oxidative desulfurization.The effects of catalyst loading,the amount of hydrogen peroxide,ionic liquid and catalyst,reaction temperature,reaction time,and different sulfur compounds on desulfurization efficiency were studied.The desulfurization rate can reach97.35%at the optimum reaction conditions:5mL of model oil,0.2mL of hydrogen peroxide,1.0mL of[BMIM]BF4,0.03g of NiW04/g-C3N4,80°C of reaction temperature and140min of reaction time.The results showed that NiW04/g-C3N4had good catalytic stability,and the catalytic activity was not significantly reduced after5repeated reactions.