工业水处理, 2021, 41(8): 7-12, 46 doi: 10.19965/j.cnki.iwt.2020-0728

• 专论与综述 •

铋基光催化剂降解四环素的研究进展

邢超,, 陈悦, 汪晟, 史静,

Research progress in the tetracycline degradation by bismuthal photocatalysts

Xing Chao,, Chen Yue, Wang Sheng, Shi Jing,

通讯作者: 史静, 副教授, E-mail: shijing_cpu@163.com

收稿日期: 2021-06-20  

基金资助: 中央高校基本科研业务费专项资金资助项目.  2632019FY02
国家自然科学基金项目.  21707166
大学生创新创业训练计划项目.  202010316067S

Received: 2021-06-20  

作者简介 About authors

邢超(1996-),硕士电话:17312273960,E-mail:1821081081@stu.cpu.edu.cn , E-mail：1821081081@stu.cpu.edu.cn

Abstract

Tetracycline(TC) is a widely used bacteriostatic agent. Its metabolism in human and animal body is not complete, can be released into the environment. In recent years, TC has been detected in water environment and soil, and its pollution has gradually attracted people's attention. Photocatalysis is one of the most effective methods to remove antibiotics. The commonly used TIO2 has some defects, such as narrow photoresponse range and easy recombination of electron-hole pair. Bismuthal photocatalysts could be used in the TC degradation in water, which had the advantages of high stability, low carrier density, and long average free path. The types and improvements of bismuthal photocatalysts were summarized. The key parameters, such as pH, TC concentration, catalyst dosage, and light intensity on TC degradation were discussed. The reaction mechanisms and the common intermediate products of TC degradation were listed. Finally, the future research direction of bismuthal photocatalyst was proposed.

Keywords： bismuthal materials ; photocatalysis ; tetracycline

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邢超, 陈悦, 汪晟, 史静. 铋基光催化剂降解四环素的研究进展. 工业水处理[J], 2021, 41(8): 7-12, 46 doi:10.19965/j.cnki.iwt.2020-0728

Xing Chao. Research progress in the tetracycline degradation by bismuthal photocatalysts. Industrial Water Treatment[J], 2021, 41(8): 7-12, 46 doi:10.19965/j.cnki.iwt.2020-0728

四环素(TC)是一种常见的抗生素〔1〕，在人体和动物体内代谢不完全，会不断释放到环境中〔2〕。许多地区的地下水、地表水及土壤中均检测出含TC的抗性菌〔3〕。

近年来，膜技术、吸附法、高级氧化技术〔4〕等方法被应用于抗生素的去除。其中，高级氧化技术中的光催化法能够高效去除抗生素〔5〕，一般使用半导体光催化剂。目前应用最多的光催化材料为TiO2，但其禁带较宽，光响应范围存在局限〔6〕。铋基化合物较为稳定，载流子密度低、平均自由程长、光催化活性较高〔7〕，可用作光催化剂，受到越来越多学者的青睐。笔者从铋基光催化剂的种类、性能改进方式、降解影响因素、光催化TC的降解产物及降解机理等方面出发，对铋基光催化材料降解TC的研究进展进行综述。

1 铋基光催化剂的种类

铋基光催化剂按元素种类可分为氧化铋、硫化铋、铋金属氧化物和铋非金属氧化物。氧化铋主要有α、β、γ、δ几种晶型，在特定条件下可相互转化〔8〕。Bi2S3的带隙较窄，光生电子-空穴的复合率较高，光催化效果较差〔9〕。铋金属氧化物由氧化铋与金属氧化物复合而成，其中Bi2WO6、Bi2MoO6、BiVO4具有优异的光催化活性，引起研究者的关注〔10-12〕。卤氧化铋是最常见的铋非金属复合氧化物之一，呈各向异性的层状结构，其光催化效率与卤素原子序数呈正比〔13〕。

铋基光催化剂根据形貌可分为片状结构〔14〕、分层结构〔15〕、空心和多孔结构〔16〕等。

2 提高铋基材料光催化性能的方法

2.1 负载

在铋基材料中掺杂元素或构成异质结结构，可增强光响应，产生等离子体效应，提高载流子分离效率等。Min Wang等〔17〕采用溶剂热合成法制备了Cu-BiVO4，Cu的掺杂使BiVO4形态发生改变，带隙变窄，光吸收增强，电子-空穴对的复合率降低。L. C. Escobar等〔18〕合成了Ag2O/BiFeO3-Ag，Ag可引起等离子体共振效应，促进光生电子-空穴对的分离，光催化活性较高。F. Opoku等〔19〕研究表明，与Bi2WO6、Bi2MoO6相比，g-C3N4/Bi2MoO6和g-C3N4/Bi2WO6的带隙均减小，载流子分离率增大。

2.2 固溶体

固溶体是在原子尺度上由2种或多种晶体杂化而成的晶态固体相。固溶体被认为是特殊的掺杂半导体，即半导体中的阴/阳离子被掺入的阴/阳离子代替。通过调节取代离子的浓度，可改变固溶体的能带结构，进而增强光催化活性。Lei Yu等〔20〕研究表明固溶体BixY1-xVO4的光催化活性受Y含量的影响。Wenqi Li等〔21〕发现微球状Bi2Mo0.4W0.6O6的光吸收率和载流子分离效率较高，其光催化活性高于Bi2 MoO6和Bi2WO6。

2.3 改变元素配比

改变元素配比可调整材料的带隙、光吸收能力和载流子分离率，进而提高光催化效率。Junping Ding等〔22〕研究表明，Bi2O2(CO3)1-xSx复合材料的配比不同时，其比表面积、电子-空穴分离率及光吸收能力有所差异。Jian Yang等〔15〕合成了三维纳米结构的BiOClxBr1-x，该材料的带隙与Br-、Cl-的配比有关。Jiankui Jia等〔23〕通过改变Bi与Ti的比例合成了不同BixTiyOz/TiO2复合物，在可见光下对TC的降解效果均优于TiO2。Jian Xu等〔24〕合成了Bi6Mo2-2xV2xO15-2x(x=0.05、0.1、0.2)材料，其带隙均小于Bi6Mo2O15带隙，x为0.2时复合材料的光催化能力最强。

3 铋基光催化剂降解TC的影响因素

3.1 pH

pH与TC的电离形态(pKa为3.3、7.7、9.7、12)、光催化剂表面电荷特性(pHzpc)密切相关〔25〕。pH可改变TC与催化剂之间的静电引力或斥力，影响铋基材料的降解能力，此外，其对系统中活性物质(·OH、e-等)的产生也有一定影响。

3.2 催化剂投加量

催化剂投加量与实验成本、催化效率有关。光照稳定时，光子在一定时间内恒定。因此，光催化过程存在最佳催化剂投加量，使催化剂能够最大程度地利用光能。当催化剂投加量小于最佳量时，光子利用率不足，TC降解效率低；催化剂投加量大于最佳量时，溶液的浊度增加，透射率降低，光催化活性受到抑制。

3.3 TC含量

在光催化体系中，TC浓度较高时降解效率较低，可能是因为高浓度的TC使得催化剂的光子吸收减少；此外，中间产物随TC初始浓度的增大而增加，加剧了TC与中间产物的竞争〔26-27〕。

3.4 光强

光催化反应速率很大程度上取决于光催化剂的辐射吸收情况。光催化过程中，光的性质或形式不影响反应途径〔28〕。光强对光降解速率的影响表现为〔29〕：低光强下，2个变量呈线性关系，这是由于电子-空穴对的形成对有机物降解起主导作用；中等光强下，由于涉及电子-空穴对的分离与重组竞争，降解速率与光强的平方根有关；高强度下，降解速率与光强无关。

表 1总结了各种影响因素下铋基材料对TC的降解情况。

表1   不同条件下铋基材料对TC的降解效果

Table 1  Degradation efficiencies of TC by bismuth-based materials under different conditions

反应体系催化剂光源影响因素最优条件TC降解率/%
光催化Bi2O7Sn2-Bi7O9I3太阳光pH: 2、6、11
催化剂: 0.5、1、1.5g/L
TC 35、55 mg/L		pH为6、
催化剂1 g/L、
TC35 mg/L		80〔30〕
光催化Bi2Sn2O7-C3N4/沸石400 W卤钨灯, 无滤光片pH: 3、6、9
催化剂: 0.75、1、1.25 g/L
TC: 10、20、30 mg/L		pH为6、催化剂1 g/L、
TC20 mg/L		80.4〔31〕
光催化Cu/Bi2Ti2O7/氧化石墨烯100 W氙灯, λ>420 nmpH: 3~10
TC: 25、50、75、100、125 mg/L		pH为7、催化剂5 g/L、
TC25 mg/L		92〔32〕
光催化Ag3PO4/AgBr/g-C3N4300 W氙灯, λ>420nmpH: 3.0、5.4、7.0、9.0
TC: 10、20、30、40、50 mg/L		pH为9.0、催化剂0.5 g/L、
TC10 mg/L		90〔26〕
光催化Sr-Bi2O3500 W氙灯, λ>420 nmpH: 3、5、7、9、11
TC: 5、10、20、50 mg/L		pH为9、催化剂0.06 g/L、
TC5 mg/L		91.2〔33〕
光催化BiOBr10 W LED灯, λ>420 nmpH: 3.1、5.1、6.2、7.3、9.1、11.0
催化剂: 0.5、1.0、1.5 g/L		pH为9.1、催化剂1.5 g/L、
TC20 mg/L		94〔34〕
光催化AgBr/Bi2WO6氙灯, λ>420 nmpH: 2、4、6、8、10
TC: 20、30、40、50、60 mg/L		pH无波动、
催化剂1 g/L、
TC20 mg/L		87.5〔27〕
光催化BiOI/Ag@AgI300 W氙灯, λ>420 nm催化剂: 0.10、0.30、0.50、1.00 g/L
TC: 20、30、40、50、60 mg/L		催化剂0.30 g/L、
TC20 mg/L		86.4〔35〕
光催化BimOnBrz400 W卤钨灯,
无滤光片		pH: 2、6、11
催化剂: 0.5、1、1.5、2 g/L
TC: 25、45 mg/L		pH为6、催化剂1 g/L、
TC25 mg/L		98.9〔36〕
光催化BiVO4/Bi2Ti2O7/Fe3O4500 W氙灯, λ>365 nmpH: 3.00、5.00、6.00、7.00、9.00
催化剂: 0.25、0.50、1.00、2.00、3.00 g/L
TC: 10、20、30、40、50 mg/L		pH为6.00、催化剂1.00 g/L、
TC10 mg/L		97.22〔37〕
光催化Bi24O31Br101 000 W氙灯, λ>420 nm催化剂: 0.5、1.0、1.5、2.0、2.5 g/L
TC: 20、40、60、80、100 mg/L		pH为4、催化剂1.5 g/L、
TC 20 mg/L		94〔38〕

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4 降解机理

4.1 半导体光催化

目前研究者普遍认为·OH、O2·-、h+、e-是光催化降解TC的主要活性物质。Bingxin Yin等〔13〕通过溶剂热法制备了Bi24O31Cl10纳米片，研究其降解TC的机理：催化剂受到光照时，e-由基态变为激发态，并从价带(VB)转移到导带(CB)；转移到CB的激发态e-与O2反应产生O2·-，进而降解TC。同时，价带中的h+可直接降解TC。Miaomiao Wu等〔39〕采用水热法合成了BiYO3纳米棒，对TC有良好的光催化活性，降解过程的主要活性物质为·OH和h+。Jinwu Bai等〔16〕通过捕获实验证明O2·-和h+是Bi2MoO6光催化氧化TC的主要活性物质。半导体光催化的降解机理如图 1(a)所示。

图1

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图1   降解机理

Fig.1   Degradation mechanisms


4.2 半导体/半导体异质结

半导体/半导体异质结一般为p-n型异质结，即光生e-从导带位置较负的半导体转移至导带位置较正的半导体导带上，而h+在价带上的流向与之相反。Ao Ren等〔40〕采用水热法合成了NiFe2O4/Bi2O3，并研究其对TC降解的光催化机理。由于NiFe2O4的CB比Bi2O3的CB更负，因此其CB中的e-会转移到Bi2O3的CB中，有利于减少电子-空穴对的复合；同时，NiFe2O4VB中的h+可直接降解TC。Juan Cheng等〔41〕制备了Bi2WO6/ZnO，对TC的降解率明显高于ZnO；捕获实验表明O2·-为光催化过程的主要活性物质。常见的半导体/半导体异质结降解TC机理如图 1(b)所示。

对于Z型异质结，光生e-从导带位置较正的半导体转移到导带位置较负的半导体价带。Yi Ma等〔42〕采用静电纺丝技术和阴离子交换法合成了Bi2S3/BiFeO3，由于形成了Z型异质结，有效提高了氧化还原效率，因此该复合材料的光催化活性远远高于Bi2S3、BiFeO3。Xiaowen Ruan等〔43〕制备了γ-Bi2MoO6/Bi12GeO20，对TC的降解速率较Bi12GeO20、Bi2MoO6分别高出约5.48、1.89倍。Z型异质结的降解机理如图 1(c)所示。

4.3 等离子体效应与导体材料掺杂

导体材料可作为e-捕获剂从而提高光催化性能。Bifu Luo等〔44〕通过光还原过程制备了Ag/Bi3TaO7等离子体光催化剂。在光照条件下，h+直接氧化OH-或H2O形成·OH，但不能形成O2·-，因为Bi3TaO7的VB电位比O2/O2·-的更正；Ag的等离子体效应可产生大量电子-空穴对，由于Bi3TaO7的CB电位比Ag的费米能级更负，因此Bi3TaO7的e-能转移到Ag并与Ag的h+结合，Ag的e-与O2产生O2·-，可氧化TC。Xingying Li等〔45〕、Enhui Jiang等〔46〕合成的Ag/Bi3.84W0.16O6.24、Ag/Bi3O4Cl复合材料光催化性能优异，得益于Ag的等离子体效应。Longfei Yue等〔47〕采用水热法合成了碳纳米管-Bi2WO6光催化剂，降解水中的TC。光生e-由Bi2WO6转移到碳纳米管中，增强了光生e-和h+的分离。与Bi2WO6相比，该复合材料的光催化活性显著提高。Jun Di等〔48〕发现多壁碳纳米管-Bi4O5Br2光催化降解TC的主要活性物质为h+和O2·-。引入导体材料降解TC的机理如图 1(d)所示。

4.4 中间产物

铋基材料降解TC过程中常见的中间产物如表 2所示。

表2   部分铋基材料降解TC过程的中间产物

Table 2  Intermediate products in TC degradation processes by some bismuth-based materials

m/z编号催化剂结构式
461A1AgBr/Bi2WO6〔27〕
CdS/Bi3O4Cl〔49〕
Cu/Bi2Ti2O7/氧化石墨烯〔32〕
BiVO4/Bi2Ti2O7〔50〕
碳掺杂氮化/Bi12O17Cl2〔51〕
BiOI/Ag@AgI〔35〕
Bi2WO6〔52〕
A2BiOBr/Bi2SiO5〔53〕
AgI/Bi2Sn2O7〔54〕
417B1AgI/Bi2Sn2O7〔54〕
Bi2WO6〔52〕
Sr-Bi2O3〔33〕
BiOBr/Bi2SiO5〔53〕
BiOI/Ag@AgI〔35〕
Ag3PO4/多壁碳纳米管/Bi2WO6〔55〕
B2Bi2MoO6〔56〕
431CAgBr/Bi2WO6〔27〕
Ag3PO4/多壁碳纳米管/Bi2WO6〔55〕
BiOI/Ag@AgI〔35〕
402D1Cu/Bi2Ti2O7/氧化石墨烯〔32〕
Bi5FeTi3O15〔57〕
BiVO4/Bi2Ti2O7〔50〕
D2AgI/Bi2Sn2O7〔54〕

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由TC的分子结构(见图 2)可知，C11a-C12处的双键及D环的电子密度较高，易受到·OH攻击，分别形成产物A1和A2。m/z 417存在2种结构：(1)C4处的—N(CH3)2去甲基化，生成产物B1；(2)C4位置受到·OH攻击脱去—N(CH3)2，同时羟基被氧化为羰基，得到产物B2。TC分子C4处的—N(CH3)2去甲基化，脱去1个CH3生成产物C(m/z 431)。TC通过2种途径得到m/z 402：(1)脱去C4处的—N(CH3)2得到产物D1；(2)脱去C2处的—CONH2，生成产物D2。

图2

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图2   TC分子结构

Fig.2   Molecular structure of TC


5 展望

采用铋基光催化剂降解水体中的TC具有稳定性高、载流子密度低、平均自由程长等优势，但也存在一些局限。未来研究应着重考虑：(1)合理设计光反应器，减少光能损失；(2)将铋基光催化剂固定在合适的载体上，实现快速分离和回收；(3)通过离子掺杂、优化异质结及构建单原子活性位点等策略，进一步增强铋基光催化剂的光降解能力；(4)对该法处理过程中的降解产物进行毒性评估，优化降解产物的生成途径，避免或减少高毒性降解产物的生成；(5)通过各表征手段进一步探究反应途径及机理，为工业化发展及应用提供理论支撑。

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