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第 35 卷第 9 期 精 细 化 工 Vol.35, No.9
201 8 年 9 月 FINE CHEMICALS Sept. 2018

催化与分离提纯技术
VO@g-C N -T 高效可见光催化苯羟基化制苯酚
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3

陈福山 1,2 ，杨 涛 1,2* ，胡华南 1,2

（1. 九江学院 化学与环境工程学院，江西 九江 332005；2. 江西省生态化工工程技术研究中心，江西 九
江 332005）

摘要：以尿素和乙酰丙酮氧钒为原料，将乙酰丙酮氧钒络合在纳米薄片石墨化氮化碳上，得到系列不同 V 质量
分数的光催化剂（VO@g-C 3 N 4 -T），将其与石墨化氮化碳（g-C 3 N 4 ）、钒氧化合物负载在石墨化氮化碳上得到的
催化剂（VO/g-C 3 N 4 ）进行了催化苯羟基化的性能对比。采用 N 2 吸附-脱附、X 射线衍射光谱（XRD）、傅里叶
变换红外光谱（FTIR）、扫描电镜（SEM）、能谱（EDS）、电感耦合等离子体-原子发射光谱（ICP-AES）对制
备的催化剂进行了表征。考察了所得催化剂可见光下催化苯羟基化制苯酚的性能。结果表明，高比表面积、纳
米薄片状的 VO@g-C 3 N 4 -T 催化剂具有合适的带差，对可见光下催化苯的 C—H 活化及羟基化具有较好的催化性
能，苯的转化率和苯酚选择性分别可以达到 98.4%、91.1%。由于石墨化氮化碳和钒具有较强的相互作用，减少
了钒的溶脱，所以该催化剂具有很好的可重复使用性，连续使用 5 次后，苯的转化率和苯酚的选择性仍然可以
达到 97.1%和 91.0%。
关键词：C—H 活化；氮化碳；光催化；多相催化剂；苯羟基化；催化技术
中图分类号：O643; O644 文献标识码：A 文章编号：1003-5214 (2018) 09-1535-07

Photocatalytic Synthesis of Phenol by Hydroxylation of Benzene over
VO@g-C 3N 4-T under Visible Light

1,2
1,2
CHEN Fu-shan , YANG Tao 1,2* , HU Hua-nan
（1. Department of Chemistry and Environment Engineering, Jiujiang University, Jiujiang 332005, Jiangxi, China;
2. Jiangxi Province Engineering Research Center of Ecological Chemical Industry, Jiujiang 332005, Jiangxi, China）

Abstract: Oxovanadium-graphitic carbon nitride thin nanosheet (VO@g-C 3N 4-T) of different V mass
fractions was prepared using urea and vanadium (Ⅳ) oxy acetylacetonate as precursors, and was compared
with graphite nitride carbon (g-C 3N 4) and oxovanadium-supported graphite nitride carbon (VO/g-C 3N 4) for
catalytic performance of benzene hydroxylation. The samples were characterized by X-ray diffraction (XRD),
Fourier translation infrared spectroscopy (FTIR), N 2 adsorption, scanning electron microscope (SEM),
energy dispersive spectroscopy (EDS), inductively coupled plasma-atomic emission spectroscopy
(ICP-AES). The photocatalytic performances of the obtained samples were tested in the hydroxylation of
benzene to produce phenol under visible light. The results showed that VO@g-C 3N 4-T nanosheets
possessed large specific surface area and had favorable bandgap, which resulted in a very good
photocatalytic activity for the hydroxylation of benzene via C−H activation under visible light. 98.4%
conversion of benzene was obtained, and the selectivity to phenol was as high as 91.1%. The good
reusability of catalyst was attributed to strong interaction between graphitic carbon nitride surface and
vanadium metal, which could minimize vanadium leaching. After being reused five times, the conversion of
benzene and the selectivity of phenol still could be up to 97.1% and 91.1%, respectively.
Key words: C-H activation; carbon nitride; photocatalysis; heterogeneous catalyst; hydroxylation of
benzene; catalysis technology
Foundation item: National Natural Science Foundation of China (21566013)

收稿日期：2017-09-22; 定用日期：2018-01-12; DOI: 10.13550/j.jxhg.20170771
基金项目：国家自然科学基金 (21566013)
作者简介：陈福山（1977—），男，讲师，博士，E-mail：93626288@qq.com。联系人：杨 涛（1977—），男，副教授，博士，电话：
0792-8314448。