Ag-BiOBr/WO<sub>3</sub>复合材料的制备及强化磺胺异噁唑去除性能

高生旺; 赵星鹏; 陆迦勒; 崔娟; 王国英; 张青

doi:10.13801/j.cnki.fhclxb.20220424.003

Ag-BiOBr/WO₃复合材料的制备及强化磺胺异噁唑去除性能

doi: 10.13801/j.cnki.fhclxb.20220424.003

高生旺^1,,
赵星鹏^{1, 2},
陆迦勒³,
崔娟^{1, 3},
王国英²,
张青^4, ,

1.
中国环境科学研究院　环境基准与风险评估国家重点实验室，北京 100012
2.
太原理工大学　环境科学与工程学院，太原 030024
3.
中北大学　理学院，先进碳基电极材料山西省重点实验室，太原 030051
4.
齐鲁工业大学　山东省科技发展战略研究所，济南 250100

基金项目: 国家重点研发计划项目(2019YFD1100201；2018YFD1100505)；中北大学创新训练项目(185)

详细信息

通讯作者:
张青，博士，高级工程师，硕士生导师，研究方向为污水处理　E-mail: xvhqing@163.com

中图分类号: X52
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- 被引次数: 0
出版历程
- 收稿日期: 2022-02-11
- 修回日期: 2022-04-13
- 录用日期: 2022-04-16
- 网络出版日期: 2022-04-25
- 刊出日期: 2023-03-15

Preparation of Ag-BiOBr/WO₃ composites and enhanced sulfisoxazole removal performance

GAO Shengwang^1
,,
ZHAO Xingpeng^{1, 2},
LU Jiale³,
CUI Juan^{1, 3},
WANG Guoying²,
ZHANG Qing^{4
, ,}

1.
State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Academy of Environmental Sciences, Beijing 100012, China
2.
School of Environmental Science and Engineering, Taiyuan University of Technology, Taiyuan 030024, China
3.
Shanxi Key Laboratory of Advanced Carbon Based Electrode Materials, School of Science, North University of China, Taiyuan 030051, China
4.
Institute of Science and Technology for Development of Shandong, Qilu University of Technology, Jinan 250100, China

Funds: National Key R&D Program Project (2019YFD1100201; 2018YFD1100505); Innovative Training Program of North University of China (185)

摘要

摘要: 抗生素类药物因其抗菌效果好在人畜医疗等领域得到广泛应用，但其在环境中难以自然分解，光催化氧化技术在降解持久型有机物方面有着光明的应用前景。然而，常规的光催化材料光谱吸收范围不够宽、光生载流子复合率过高，严重制约了催化材料的应用推广。因此，亟待研发更有效安全的去除技术。本文利用光沉积法将Ag单质负载于BiOBr/WO₃ p-n型异质结材料表面，构建出新型Ag-BiOBr/WO₃材料，并将其用于光催化降解磺胺异噁唑。采用XRD、TEM、XPS、UV-vis DRS等技术对其进行表征表明，Ag的沉积拓展了材料的光响应范围，显著加快光生载流子的分离速度，从而提高了光催化性能。单质Ag含量为15wt%的材料为降解磺胺异噁唑效率最高的复合材料。当溶液中催化剂浓度为0.3 g/L，磺胺异噁唑浓度为5 mg/L，pH为7时，在60 min时光催化降解磺胺异噁唑的效率最高，可达98.1%，降解速率常数分别为BiOBr、WO₃和BiOBr/WO₃的28.79倍、36.37倍和7.59倍。经过5次循环实验后，15wt%Ag-BiOBr/WO₃复合材料仍具备较高的光催化活性，表明材料可循环回收利用，具备良好的稳定性。淬灭实验和电子自旋共振(ESR)结果表明，•O₂^–为15wt%Ag-BiOBr/WO₃体系中最活跃的自由基团，而¹O₂和h⁺发挥了次要作用。这为催化材料的制备和抗生素降解提供了理论基础。
- 磺胺异噁唑 /
- 光催化技术 /
- 溴氧化铋 /
- 三氧化钨 /
- 银
Abstract: Antibiotics have been widely used to treat human and animal diseases with good antibacterial effect. However, antibiotics are difficult to be degraded naturally in natural environment. The photocatalytic oxidation technology has bright application prospects in the degradation of persistent organic compounds. However, the spectral absorption range of conventional photocatalytic materials is not wide enough, and the recombination rate of photogenerated carriers is too high, which seriously restricts the application and promotion of catalytic materials. So, it is urgent to develop more effective and safe removal technologies. The photodeposition method was used to load Ag element on the surface of BiOBr/WO₃ p-n type heterojunction material to construct a new type of Ag-BiOBr/WO₃ material and apply to the photocatalytic degradation of sulfisoxazole. The samples were characterized by various techniques, such as XRD, TEM, XPS, UV-vis DRS et al. The result show that the deposition of Ag expands the photo-response range of the material, significantly accelerates the separation speed of photogenerated carriers, and thus improves the photocatalytic performance. The 15wt%Ag-BiOBr/WO₃ with an Ag content of 15wt% is considered to be the most efficient composite material for the removal of sulfisoxazole. When the catalyst concentration is 0.3 g/L, the sulfisoxazole concentration is 5 mg/L, and the pH is 7, 15wt%Ag-BiOBr/WO₃ demonstrates the highest photocatalytic degradation efficiency of sulfisoxazole in 60 min, which reaches up to 98.1%. The degradation rate is 28.79, 36.37 and 7.59 times higher than those of BiOBr, WO₃ and BiOBr/WO₃, respectively. After 5 cycles of experiments, the 15wt%Ag-BiOBr/WO₃ composite material still maintains high photocatalytic activity, indicating that the material can be recycled and reuses with good stability. The quenching experiments and electron spin resonance (ESR) shows that •O₂^– is the most active radical group in the BiOBr/WO₃ system, while ¹O₂ and h⁺ played relatively minor roles. This provides a theoretical basis for the preparation of catalytic materials and the degradation of antibiotics.
- sulfisoxazole /
- photocatalytic technology /
- bismuth bromide oxide /
- tungsten trioxide /
- silver

HTML全文

图 1 Ag-BiOBr/WO₃复合材料的XRD图谱

Figure 1. XRD spectra of Ag-BiOBr/WO₃ composite

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图 2 15wt%Ag-BiOBr/WO₃的XPS图谱：(a) 总谱；(b) Bi4f；(c) Br3d; (d) O1s；(e) W4f; (f) Ag3d

Figure 2. XPS spectra of 15wt%Ag-BiOBr/WO₃: (a) Full spectra; (b) Bi4f; (c) Br3d; (d) O1s; (e) W4f; (f) Ag3d

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图 3 BiOBr (a)、WO₃(b)、BiOBr/WO₃(c) 和15wt%Ag-BiOBr/WO₃(d) 的SEM图像；(e) 15wt%Ag-BiOBr/WO₃的TEM图像；(f) 15wt%Ag-BiOBr/WO₃的HRTEM图像

Figure 3. SEM images of BiOBr (a), WO₃ (b), BiOBr/WO₃ (c) and 15wt%Ag-BiOBr/WO₃ (d); (e) TEM image of 15wt%Ag-BiOBr/WO₃; (f) HRTEM image of 15wt%Ag-BiOBr/WO₃

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图 4 15wt%Ag-BiOBr/WO₃的元素面扫图及EDS能谱图

Figure 4. Element surface scan and EDS spectrum of 15wt%Ag-BiOBr/WO₃

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图 5 复合材料的氮气吸附-脱附等温线(插图为孔径分布曲线)

Figure 5. Nitrogen adsorption-desorption isotherms of composite materials (Inset is the pore size distribution curves)

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图 6 复合催化剂对磺胺异噁唑的降解曲线 (a) 和反应动力学 (b)

Figure 6. Degradation curves (a) and reaction kinetics (b) of sulfisoxazole by composite catalyst

C₀—Initial concentration of the degradation substrate; C_t—Concentration at the t time of the degradation substrate

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图 7 不同投加量 (a) 和反应初始浓度 (b) 对15wt%Ag-BiOBr/WO₃催化性能的影响；(c) 15wt%Ag-BiOBr/WO₃的Zeta 电位

Figure 7. Different dosage (a) and influence of initial reaction concentration (b) on the catalytic performance of 15wt%Ag-BiOBr/WO₃; (c) Zeta potential of 15wt%Ag-BiOBr/WO₃

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图 8 所制备催化剂的电化学阻抗图谱 (a)、光电流响应 (b) 和荧光图谱 (c)

Figure 8. Electrochemical impedance spectra (a), photocurrent response (b) and fluorescence spectra (c) of the prepared material

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图 9 Ag-BiOBr/WO₃复合材料的紫外-可见漫反射光谱图和(αhv)²和hv的关系曲线(插图)

Figure 9. Ultraviolet-visible diffuse reflectance spectra of the Ag-BiOBr/WO₃ composite and the relationship curve between (αhv²) and hv (Inset)

α—Absorption coefficient; h—Planck constant; v—frequency

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图 10 (a) 15wt%Ag-BiOBr/WO₃降解磺胺异噁唑(SSX)过程中的自由基捕获实验(浓度[SSX]=5 mg/L、[15wt%Ag-BiOBr/WO₃]=0.3 g/L); (b) ¹O₂和•O₂^–的电子顺磁共振检测

Figure 10. (a) Free radical capture experiment in the process of 15wt%Ag-BiOBr/WO₃ degradation of sulfisoxazole (SSX) (Concentration [SSX]=5 mg/L, [15wt%Ag-BiOBr/WO₃]=0.3 g/L); (b) Electron paramagnetic resonance detection of ¹O₂ and •O₂^–

IPA—Isopropanol; EDTA-2Na—Disodium ethylene diamine tetraacetic acid; BQ—Benzoquinone

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图 11 15wt%Ag-BiOBr/WO₃在可见光照射下的光催化反应机制

Figure 11. Photocatalytic reaction mechanism of 15wt%Ag-BiOBr/WO₃ under visible light irradiation

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图 12 15wt%Ag-BiOBr/WO₃对光催化降解磺胺异噁唑的回收利用实验

Figure 12. Recycling experiment of 15wt%Ag-BiOBr/WO₃ for photocatalytic degradation of sulfisoxazole

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表 1 Ag-BiOBr/WO₃复合材料比例

Table 1. Proportion of Ag-BiOBr/WO₃ composites

Specimen	Mass fraction of Ag/wt%
BiOBr/WO₃	0
1wt%Ag-BiOBr/WO₃	1
5wt%Ag-BiOBr/WO₃	5
10wt%Ag-BiOBr/WO₃	10
15wt%Ag-BiOBr/WO₃	15
20wt%Ag-BiOBr/WO₃	20

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表 2 氮气吸附-脱附法测定复合材料比表面积

Table 2. Nitrogen adsorption-desorption method to determine the specific surface area of composite materials

Sample	Specific surface area/(m²·g^–1)	Pore volume/ (cm³·g^–1)	Average pore size/nm
WO₃	6.5917	0.0088	5.3087
BiOBr	12.4277	0.0158	5.0858
BiOBr/WO₃	13.6590	0.0685	20.5770
15wt%Ag-BiOBr/WO₃	9.0180	0.0431	19.1025

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