水解剂氟化铵对Fe-SBA-15结构及催化性能的影响

doi:10.11962/1006-4990.2018-0562

摘要/Abstract

摘要：

通过水热法制备了Fe-SBA-15介孔材料,探究了水解剂氟化铵对介孔材料结构及对苯酚羟基化反应的影响。采用X射线衍射（XRD）、红外光谱（FT-IR）和氮气吸附-脱附等方法对介孔材料进行了表征,用苯酚羟基化反应对改性后介孔材料的催化性能进行了研究。结果表明:改性后的介孔材料具有良好的催化性能,其中氟与硅物质的量比为0.03时制备的介孔材料的催化性能更为优良,在固定反应条件下苯酚转化率达到36.82%、苯二酚选择性达到81.76%。

关键词: 水解剂, 氟化铵, Fe-SBA-15, 苯二酚, 羟基化

Abstract:

Fe-SBA-15 mesoporous materials were prepared by hydrothermal synthesis,and the effect of hydrolysis agent NH₄F on the mesoporous materials structure and catalytic hydroxylation of phenol was explored.The mesoporous materials were characterized by X-ray diffraction（XRD）,infrared spectroscopy（FT-IR） and N₂ adsorption desorption etc..The catalytic properties of modified mesoporous materials were studied by hydroxylation of phenol.The results indicated that the modified materials had good catalytic performance.When n（F^-）/n（Si）=0.03,the prepared mesoporous materials had better catalytic performance.Under the fixed reaction conditions,conversion of phenol and selectivity of dihydroxybenzene reached 36.82% and 81.76%,respectively.

Key words: hydrolysate, NH₄F, Fe-SBA-15, dihydroxybenzene, hydroxylation

中图分类号:

O643

邵艳秋,张宇婷,姜振双,刘素娟,任玉兰,王丽杰. 水解剂氟化铵对Fe-SBA-15结构及催化性能的影响[J]. 无机盐工业, 2019, 51(9): 97-101.

Shao Yanqiu,Zhang Yuting,Jiang Zhenshuang,Liu Sujuan,Ren Yulan,Wang Lijie. Effects of hydrolysate NH₄F on structure and catalytic properties of Fe-SBA-15[J]. Inorganic Chemicals Industry, 2019, 51(9): 97-101.

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样品	比表面积/ （m²·g^-1）	孔体积/ （cm³·g^-1）	平均孔直径/ nm
SBA-15	880.84	1.57	7.94
Fe-SBA-15	843.44	1.14	5.39
Fe-SBA-15（0.01）	833.61	1.47	6.44
Fe-SBA-15（0.02）	783.44	1.32	6.67
Fe-SBA-15（0.03）	681.11	1.30	6.76
Fe-SBA-15（0.04）	699.96	1.47	6.82
Fe-SBA-15（0.05）	764.58	1.84	7.22

样品	[n（Fe）/n（Si）]/%		嫁接率/ %
样品	理论值	实际值	嫁接率/ %
Fe-SBA-15	5	2.37	47.4
Fe-SBA-15（0.01）	5	2.89	57.8
Fe-SBA-15（0.02）	5	3.04	60.8
Fe-SBA-15（0.03）	5	3.22	64.4
Fe-SBA-15（0.04）	5	2.51	50.2
Fe-SBA-15（0.05）	5	2.19	43.8

催化剂	苯酚转化率/%	邻苯二酚选择性/%	对苯二酚选择性/%
SBA-15	1.35	—	—
Fe-SBA-15	23.61	37.25	29.73
Fe-SBA-15（0.01）	29.56	38.76	31.75
Fe-SBA-15（0.02）	33.17	40.13	32.63
Fe-SBA-15（0.03）	36.82	45.51	36.25
Fe-SBA-15（0.04）	21.47	19.70	11.57
Fe-SBA-15（0.05）	18.10	10.55	8.14

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