PI-g-C3N4光催化剂的制备及其光催化降解苯酚性能

doi:10.16085/j.issn.1000-6613.2025-0259

摘要/Abstract

摘要：

采用热聚合法制备了苝四羧酸二酐（PTCDA）修饰的石墨相氮化碳（g-C₃N₄）光催化剂（PI-g-C₃N₄），并研究其光催化降解苯酚（phenol，缩写为Ph）的效果及其可能的光催化反应机制。采用扫描电子显微镜（SEM）、透射电子显微镜（TEM）、X射线衍射（XRD）、傅里叶变换红外吸收光谱（FTIR）、X射线光电子能谱仪（XPS）、UV-Vis漫反射光谱（UV-Vis-DRS）、光电流分析、莫特-肖特基（Mott-Schottky，M-S）曲线等方法对制备的PI-g-C₃N₄光催化剂进行表征。考察了不同催化剂、催化剂投加量、不同溶液初始pH、不同实际水体对光催化降解Ph的影响。结果表明，当利用氙灯（配置波长大于400nm的滤光片）作为光源，催化剂PI-g-C₃N₄投加量为1.0g/L、污染物Ph初始浓度为10mg/L、反应120min时，Ph的去除率可达91%，且降解Ph的速率常数为0.02min^-1，是单独g-C₃N₄或PTCDA降解Ph的10倍和250倍。催化剂投加量和碱性条件均有利于Ph的降解。自由基淬灭实验和电子自旋共振实验结果证明，该体系中光生空穴（h⁺）、超氧自由基（O₂^•-）和过氧化氢（H₂O₂）是降解Ph的主要活性物种。PI-g-C₃N₄为S型异质结构，通过π-π共轭相互作用将PTCDA与g-C₃N₄结合，有效促进了光生电子-空穴对的分离，实现了光催化降解Ph的性能提升。最后，催化剂循环利用实验证明了制备的PI-g-C₃N₄光催化剂具有较好的重复利用性。本研究旨在为光催化材料在环境污染治理领域提供新思路和新方法。

关键词: 光催化, 石墨相氮化碳, 苝四羧酸二酐, 苯酚降解

Abstract:

In this study, a perylene tetracarboxylic dianhydride (PTCDA)-modified graphitic carbon nitride (g-C₃N₄) composite photocatalyst (PI-g-C₃N₄) was synthesized via thermal polymerization. The photocatalytic degradation efficiency of phenol (Ph) via PI-g-C₃N₄/Vis system and its possible reaction mechanism were systematically investigated. The prepared PI-g-C₃N₄ composite photocatalyst was characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), UV-Vis diffuse reflectance spectroscopy (UV-Vis-DRS), transient photocurrent response analysis and Mott-Schottky (M-S) plots. The effects of different catalysts, catalyst dosages, initial solution pH and different actual water backgrounds on the photocatalytic degradation of Ph were evaluated. The results demonstrated that under xenon lamp irradiation (with a filter for λ>400nm) with a PI-g-C₃N₄ dosage of 1.0g/L, an initial Ph concentration of 10mg/L and a reaction time of 120min, the removal efficiency of Ph reached 91% with a degradation rate constant of 0.02min^-1, which was 10 times and 250 times of Ph degradation by g-C₃N₄ or PTCDA alone. The dosage of catalyst and alkaline condition were all favorable for Ph degradation. Radical quenching experiments and electron spin resonance (ESR) analysis revealed that photogenerated holes (h⁺), superoxide radicals (O₂^•-) and hydrogen peroxide (H₂O₂) were the primary active species responsible for Ph degradation. PI-g-C₃N₄ was an S-scheme heterostructure, where PTCDA was coupled with g-C₃N₄ through π-π conjugation interactions. This configuration effectively facilitated the separation of photogenerated electron-hole pairs, ultimately leading to significant enhancement in photocatalytic degradation performance for Ph. Furthermore, recycling experiments confirmed the excellent reusability of the PI-g-C₃N₄ composite catalyst. This study provided new insights and methodologies for the application of photocatalytic materials in environmental pollution control.

Key words: photocatalysis, graphitic carbon nitride, perylene tetracarboxylic dianhydride, phenol degradation

中图分类号:

张娟娟, 凌裕, 黎佳茜, 刘雪瑜. PI-g-C₃N₄光催化剂的制备及其光催化降解苯酚性能[J]. 化工进展, 2025, 44(10): 6102-6114.

ZHANG Juanjuan, LING Yu, LI Jiaxi, LIU Xueyu. Preparation of PI-g-C₃N₄ photocatalyst and its photocatalytic degradation performance of phenol[J]. Chemical Industry and Engineering Progress, 2025, 44(10): 6102-6114.

图/表 20

图1 PI-g-C3N4的合成路线

图2 g-C3N4、PTCDA、PI-g-C3N4的照片、SEM及TEM图像

图3 g-C3N4、PTCDA、PI-g-C3N4的XRD谱图

图4 g-C3N4、PTCDA、PI-g-C3N4的FTIR谱图

图5 g-C3N4、PTCDA、PI-g-C3N4的XPS谱图

图6 g-C3N4、PTCDA、PI-g-C3N4的UV-Vis谱图

图7 g-C3N4、PTCDA、PI-g-C3N4在0V（vs. SCE）下的瞬态光电流响应

图8 在黑暗条件下测得的g-C3N4和PI-g-C3N4的Mott-Schottky图

图9 不同催化剂g-C3N4、PTCDA、PI-g-C3N4对Ph的吸附性能

图10 不同催化剂g-C3N4、PTCDA、PI-g-C3N4对Ph光催化降解的影响

图11 不同催化剂g-C3N4、PTCDA、PI-g-C3N4对Ph光催化降解TOC去除率的影响

表1 不同光催化材料对比分析表

催化剂类型	改性策略	降解率/%	反应时间/min	速率常数/min^-1	主要改进机制	参考文献
PI-g-C₃N₄	PTCDA与g-C₃N₄酰胺反应复合	91	120	0.020	S型电荷传输，增强界面电荷分离	本研究
CoPC/g-C₃N₄	金属掺杂	82	240	0.015	窄化带隙，提升光响应范围	[44]
S/g-C₃N₄	非金属掺杂	56	90	0.009	窄化带隙，提升光响应范围	[45]
Bi₂O₃/g-C₃N₄	异质结复合	36.6	75	0.006	促进光生电子-空穴对分离	[46]

图12 催化剂PI-g-C3N4投加量对Ph光催化降解的影响

图13 催化剂PI-g-C3N4体系中溶液初始pH对Ph光催化降解的影响

图14 催化剂PI-g-C3N4体系在不同水体中对Ph光催化降解的影响

图15 催化剂PI-g-C3N4体系中不同淬灭剂对Ph光催化降解的影响

图16 采用DMPO和BMPO作为捕获剂的·OH和O2•-的ESR光谱

图17 可见光照射下提出的PI-g-C3N4的两种电荷分离模型

图18 PI-g-C3N4/Vis体系中Ph降解的可能光催化机制

图19 PI-g-C3N4/Vis体系中Ph降解的循环实验

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PI-g-C₃N₄光催化剂的制备及其光催化降解苯酚性能

Preparation of PI-g-C₃N₄ photocatalyst and its photocatalytic degradation performance of phenol

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