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石墨烯基金属硫化物复合物的制备及其光催化降解环丙沙星的性能研究
论文作者:童鞋论文网  论文来源:www.txlunwenw.com  发布时间:2019/9/9 8:43:39  

摘要:环丙沙星(CIP)作为一种光谱抗生素被广泛的运用于临床医学治疗,然而CIP的大量使用造成水体中抗生素残留严重,对生态环境的影响极大。近年来,光催化技术因其无毒廉价等优势被广泛运用于解决水体污染问题。其中,石墨烯基金属硫化物光催化剂因其优异的催化性能受到研究者广泛的研究。本文以金属硫化物(ZnS、CdS)为主体,引入Cu2+进行的掺杂以扩宽其光响应范围,同时使用石墨烯作为载体,制得复合光催化剂。通过X射线衍射仪(XRD)、傅里叶变换红外光谱(FTIR)、扫描电子显微镜(SEM)、透射电镜(SEM)、紫外可见吸收光谱(UV-Vis)等方法对复合光催化剂进行表征分析,并测试该光催化剂对CIP的降解效率,具体内容如下:

(1) 通过一步水热法制备了光催化剂CuxZn1-xS/RGO,同步实现了CuxZn1-xS纳米颗粒的可控生长和氧化石墨烯(GO)的还原。结果表明,石墨烯的引入有效地抑制了纳米粒子的团聚,直径约为20 nm的颗粒状CuxZn1-xS均匀分布在石墨烯片层上。紫外可见光谱分析显示,在掺杂了Cu2+后,该光催化剂的可见光响应范围扩宽至可见光区域,为可见光光催化研究提供了可能。对复合物制备条件进行了优化,发现当铜锌比为1:10,石墨烯负载量为10 wt%时,CuxZn1-xS/RGO复合物的光催化性能最佳,在3 h内对10 mg/L CIP的降解率达到了90%,降解效率分别是ZnS、Cu0.1Zn0.9S的4.5倍和3倍,说明金属硫化物和石墨烯之前存在协同效应,石墨烯的引入能有效提高复合物的可见光催化性能,且对ZnS光催化性能的提升要更为明显。此外,反应机理研究表明,在该光催化反应过程中共有三种自由基参与了反应,其中•O2-起主导作用,h+和•OH起次要作用。

(2) 通过一步水热法制备了光催化剂CuxCd1-xS/RGO,并将其应用于对CIP的光催化降解。结果表明,直径为10-20 nm的颗粒状CdxZn1-xS均匀密布在石墨烯片层上,石墨烯的引入有效的抑制了纳米粒子的团聚,也使得石墨烯片层分散开来,不易堆叠在一起。紫外可见光谱分析显示,在掺杂了Cu2+后,该光催化剂的光响应范围扩宽至可见光区域;在复合了石墨烯后,光催化剂的光响应值又有了明显的提升,这为可见光光催化研究提供了可能。对复合物的制备进行了优化,发现当铜镉比为1:20,石墨烯负载量为5 wt%时,Cu0.05Cd0.95S/RGO5复合物具有最为优异的光催化性能,10 mg光催化剂在3 h内对50 ml的10 mg/L CIP的降解率为94%,降解效率分别为CdS和Cu0.5Cd0.95S的4倍和3.4倍,说明金属硫化物和石墨烯之间存在协同效应,使光生电子能更好的转移,石墨烯的引入能够有效的提升光催化剂的可见光光催化性能,且对CdS光催化性能的提升更为明显。且在循环使用5次后依然有90%以上的降解率,具有良好的稳定性。此外,机理实验表明,在该光催化反应过程中•O2-、h+和•OH这三种自由基均参与了反应,其中•OH起主导作用,h+和•O2-起次要作用。

Ciprofloxacin (CIP) is widely used as akind of spectroscopic antibiotics in clinical medical treatment. However, theextensive use of CIP causes serious antibiotic residues in water bodies and hasa great impact on the ecological environment. In recent years, photocatalytictechnology has been widely used to solve water pollution problems because ofits advantages such as non-toxicity and low cost. Among them, the graphenemetal sulfide photocatalyst has been extensively studied by researchers becauseof its excellent catalytic performance. In this paper, metal sulfide (ZnS, CdS)is the main body, and Cu2+ is doped to broaden its photoresponse range. At thesame time, graphene is used as a carrier to prepare a composite photocatalyst.The composite photocatalyst was characterized by X-ray Diffraction (XRD),Fourier Transform Infrared Spectrum (FTIR), Scanning Electron Microscope (SEM),Transmission Electron Microscope (SEM), Ultraviolet-Visible Absorption Spectrum(UV-Vis) and other methods, and the degradation efficiency of CIP was tested.The details are as follows:

(1) The photocatalyst CuxZn1-xS/RGO wasprepared by one-step hydrothermal method, and the controlled growth ofCuxZn1-xS nanoparticles and the reduction of graphene oxide (GO) weresimultaneously realized. The results show that the combination of grapheneeffectively inhibits the agglomeration of nanoparticles, and the granularCuxZn1-xS with a diameter of about 20 nm is uniformly densely coated on thegraphene sheets. UV-visible spectroscopy analysis showed that the visible lightresponse range of the photocatalyst was broadened to visible light after dopingwith Cu2+, which provided a possibility for visible light photocatalysis. Thepreparation conditions of the composites were optimized. It was found that whenthe amount of graphene compounded was 10 wt% and the ratio of copper to zincwas 1:10, the photocatalytic performance of the composite photocatalyst was thebest, and 10 mg/L was obtained within 3 h. The degradation rate of CIP solutionreached 90%, which was 4.5 times and 3 times that of ZnS and Cu0.1Zn0.9S,respectively. This indicates that there is a synergistic effect between metalsulfide and graphene. The composite of graphene can effectively improve thevisible light catalysis of the composite. Performance, and the improvement ofZnS photocatalytic performance is more obvious. In addition, reaction mechanismstudies have shown that three kinds of free radicals participate in thereaction during the photocatalytic reaction, in which •O2- plays a dominantrole, and h+ and •OH play a secondary role.

(2) The photocatalyst CuxCd1-xS/RGO wasprepared by a simple one-step hydrothermal method and applied to thephotocatalytic degradation of CIP. The results show that the granular CdxZn1-xSwith a diameter of 10-20 nm is uniformly densely coated on the graphene sheet.The combination of solid graphene effectively inhibits the agglomeration of thenanoparticles and also makes the graphene sheets dispersed and difficult tostack. Together. UV-visible spectroscopy analysis showed that thephoto-response range of the photocatalyst was broadened to the visible lightregion after doping with Cu2+. After the graphene was compounded, thephoto-response value of the photocatalyst was significantly improved. Catalyticresearch offers the possibilities. The preparation of the composite wasoptimized. It was found that when the ratio of copper to cadmium was 1:20 andthe ratio of graphene was 5 wt%, Cu0.05Cd0.95S/RGO5 had the most excellentphotocatalytic performance, and 10 mg of photocatalyst was in 3 The degradationrate of 50 ml of 10 mg/L CIP solution was 94% in h, which was 4 times and 3.4times higher than that of CdS and Cu0.5Cd0.95S, respectively, indicating thatthere is a synergistic effect between metal sulfide and graphene.

关键词:金属硫化物;光催化;环丙沙星;石墨烯

Metal sulfides; Photocatalysis;Ciprofloxacin; Graphene

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