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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。
Hydrothermal synthesis of NiWO_4 nanoparticles, and then by mixed calcination method successfully prepared supported catalyst NiWO_4 / g-C_3N_4. The morphology and structure of NiWO_4 / g-C_3N_4 were characterized by XRD, FT-IR, EDS, SEM, BET and XPS. NiWO_4 / g-C_3N_4 as catalyst, hydrogen peroxide as oxidant and 1-butyl-3-methylimidazolium tetrafluoroborate ionic liquid ([BMIM] BF4) as extractant. The influence of the amount of catalyst, hydrogen peroxide, ionic liquid and catalyst, reaction temperature, reaction time and different kinds of sulfur compounds on the desulfurization effect were investigated. The results showed that the optimum reaction conditions were as follows: 5 m L of simulated oil, 0.2 m L hydrogen peroxide, 1.0 m L [BMIM] BF 4, 0.03 g NiWO 4 / g-C 3 N 4, reaction temperature 80 ℃ and reaction time 140 min Under the reaction conditions, the desulfurization rate can reach 97.35%. The experimental results show that NiWO 4 / g-C 3 N 4 has good catalytic stability, and the catalytic activity of NiWO 4 / g-C 3 N 4 is not significantly reduced after being repeatedly used for five times.