g-C_(3)N_(5)/MoO_(3)复合材料的制备及其电化学检测与光催化降解对乙酰氨基酚  

Preparation of g-C_(3)N_(5)/MoO_(3) composite material and its application in electrochemical detection and photocatalytic degradation of acetaminophen

作　　者：王晓云 付爱民 WANG Xiaoyun;FU Aimin(School of Ecological Environment and Urban Construction,Fujian University of Technology,Fuzhou 350008;Fujian Ningde Nuclear Power Company Limited,Ningde 355200)

机构地区：[1]福建理工大学生态环境与城市建设学院,福州350008 [2]福建宁德核电有限公司,宁德355200

出　　处：《环境科学学报》2024年第12期91-104,共14页Acta Scientiae Circumstantiae

摘　　要：采用超声-共沉淀法制备了一系列不同质量比例g-C_(3)N_(5)的g-C_(3)N_(5)/MoO_(3)复合材料,并采用XRD、UV-Vis DRS、FTIR、XPS、SEM和TEM等方法研究了材料的结构和光学性能.以g-C_(3)N_(5)/MoO_(3)修饰玻碳电极表面构建了对乙酰氨基酚(AAP)电化学传感器,交流阻抗法、循环伏安法和差动脉冲伏安法的结果显示,10%g-C_(3)N_(5)/MoO_(3)修饰电极对AAP具有良好的电催化氧化活性.将此传感器用于检测AAP,线性范围为5~1540μmol·L^(-1),灵敏度为0.523μA·μmol^(-1)·L·cm^(-2),检测限为3 nmol·L^(-1)(S/N=3).此传感器具有优异的抗干扰性能、良好的重现性和高稳定性,用于实际样品中APP的检测,加标回收率为98.52%~101.06%,RSD<3.50%.在可见光条件下(光功率为50 W),10%g-C_(3)N_(5)/MoO_(3)在120 min内对100μmol·L^(-1)AAP的降解率为99.5%.通过自由基猝灭实验和顺磁电子共振测试发现,在光催化体系中的主要活性物质为·OH和·O_(2)^(-),其次为h^(+),并提出了可能的降解机理.复合材料连续10次循环使用后对AAP的去除率仍然达到93.22%,说明材料具有较好的使用寿命.A series of g-C_(3)N_(5)/MoO_(3) composite materials with different mass ratios of g-C_(3)N_(5) were prepared by an ultrasonic-coprecipitation method.The structural and optical properties of these materials were investigated by XRD,UV-Vis DRS,FTIR,XPS,SEM,and TEM.An electrochemical sensor for acetaminophen(AAP)was constructed on a glassy carbon electrode modified with g-C_(3)N_(5)/MoO_(3).The results of electrochemical impedance spectroscopy(EIS),cyclic voltammetry(CV),and differential pulse voltammetry(DPV)showed that the 10%g-C_(3)N_(5)/MoO_(3) modified electrode has good electrocatalytic oxidation activity for AAP.When using this sensor for AAP detection,the linear range was 5~1540μmol·L^(-1),the sensitivity was0.523μA·μmol^(-1)·L·cm^(-2),and the detection limit was 3 nmol·L^(-1)(S/N=3).The sensor exhibited excellent anti-interference performance,good reproducibility,and high stability.It was applied to detect AAP in actual samples with recoveries between 98.52%~101.06%and RSD<3.50%.Under visible light conditions(50 W),10%g-C_(3)N_(5)/MoO_(3) could degrade 99.5%of AAP(100μmol·L^(-1))within 120 min.Free radical quenching experiments and electron paramagnetic resonance tests revealed that·OH and·O_(2)^(-)were the main active species in the photocatalytic system,followed by h^(+).A possible degradation mechanism was proposed.After 10 consecutive cycles,the removal rate of AAP by the composite material still reached 93.22%,indicating that the material has a good service life.

关 键 词：g-C_(3)N_(5)/MoO_(3) 电化学检测 光催化降解 对乙酰氨基酚 

分 类 号：X703[环境科学与工程—环境工程]