二次等温热缩聚改性对g-C3N4光催化剂性能的影响

doi:10.16085/j.issn.1000-6613.2020-1305

化工进展 ›› 2021, Vol. 40 ›› Issue (6): 3389-3400.DOI: 10.16085/j.issn.1000-6613.2020-1305

二次等温热缩聚改性对g-C₃N₄光催化剂性能的影响

段丽媛¹^,²(), 李国强¹^,²(), 张舒婷¹^,², 王宏宇¹^,², 赵永乐¹^,², 张永发¹^,²

^1.太原理工大学省部共建煤基能源清洁高效利用国家重点实验室，山西太原 030024
^2.太原理工大学煤科学与技术教育部重点实验室，山西太原 030024

收稿日期:2020-07-10 修回日期:2020-11-12 出版日期:2021-06-06 发布日期:2021-06-22
通讯作者: 李国强
作者简介:段丽媛（1996—），女，硕士研究生，研究方向为光催化。E-mail：136487953@qq.com。
基金资助:
山西省煤基重点攻关项目(MJH2014-09);山西省重点研发项目(201703D321006);太原理工大学青年基金(2015QN093)

Effect of secondary isothermal condensation modification on the performance of g-C₃N₄ photocatalyst

DUAN Liyuan¹^,²(), LI Guoqiang¹^,²(), ZHANG Shuting¹^,², WANG Hongyu¹^,², ZHAO Yongle¹^,², ZHANG Yongfa¹^,²

^1.State Key Laboratory of Clean and Efficient Coal Utilization, Taiyuan University of Technology, Taiyuan 030024, Shanxi, China
^2.Key Laboratory of Coal Science and Technology, Ministry of Education, Taiyuan University of Technology, Taiyuan 030024, Shanxi, China

Received:2020-07-10 Revised:2020-11-12 Online:2021-06-06 Published:2021-06-22
Contact: LI Guoqiang

摘要/Abstract

摘要：

采用二次等温热缩聚方式对通过NH₄SCN制得的g-C₃N₄进行处理，通过XRD和SEM/TEM等手段对所制备样品的物相结构、表面形貌等结构特性及有机染料RhB的降解效果进行了研究。结果表明，二次等温热缩聚改性使催化剂聚合度增加，层间距缩短，通过调节等温热缩聚处理时间构建了蜂窝孔洞薄片层表面结构，比表面积和孔容积分别增加了2.3倍和4.7倍；大量—NH—、—NH₂等氨基基团的产生，带来了更高的吸附氧含量；带隙宽度由2.77eV拓宽至2.81eV，且价带位置增至+1.625eV，使光生空穴拥有更强的氧化降解能力；边缘三嗪环结构单元中C—N $? ????$ C位置上N元素缺失，减少了大量光生电荷的复合消耗，PL荧光光谱显示了明显降低的光生电子-空穴复合率，对载流子的充分利用使催化速率明显提高。有机污染物RhB催化降解效果显著，光催化反应速率常数由0.006提高到0.031，反应速率提高了5.2倍，在420nm可见光下照射90min，降解率由42%提高至98%。

关键词: 光化学, 催化, 降解, 石墨相氮化碳, 二次等温热缩聚, 氮空位, 蜂窝孔洞薄片层

Abstract:

g-C₃N₄, a semiconductor photocatalyst, was successfully prepared from NH₄SCN by thermal polymerization and was modified by secondary isothermal condensation. The phase structure and surface morphology of the product sample were characterized by XRD and SEM/TEM, and the photocatalyst activity was evaluated by degradation of the organic dye RhB. The results showed that the polymerization degree of the catalyst was increased and the layer spacing was shortened by secondary isothermal condensation modification. With the adjustment of isothermal condensation treatment time, the specific surface area and pore volume increased by 2.3 times and 4.7 times, respectively. In addition, a large number of amino groups, such as —NH—and —NH₂, resulted in a higher adsorption capacity of oxygen. The band gap width of the catalyst samples was widened from 2.77eV to 2.81eV after secondary isothermal condensation modification, the position of the valence band also increased to +1.625eV, and the photo-cavitation oxidation degradation ability was enhanced. There were N defects in the C—N $? ????$ C position of the edge triazine rings, which significantly reduced the consumption of the photogenerated charges. At the same time, the intensity of the emission peak of the fluorescence spectrum decreased significantly, indicating that the photoelectron-hole binding rate decreased, and the effective utilization of the carrier significantly increased the catalytic reaction rate. After the irradiation under 420nm visible light for 90 min, the photocatalytic reaction rate constant increased from 0.006 to 0.031, the reaction rate increased by 5.2 times, and the degradation rate increased from 42% to 98%.

Key words: photochemical, catalytic, degradation, graphitic carbon nitride (g-C₃N₄), secondary isothermal condensation, nitrogen space, honeycomb orifice laminate

中图分类号:

X703

段丽媛, 李国强, 张舒婷, 王宏宇, 赵永乐, 张永发. 二次等温热缩聚改性对g-C₃N₄光催化剂性能的影响[J]. 化工进展, 2021, 40(6): 3389-3400.

DUAN Liyuan, LI Guoqiang, ZHANG Shuting, WANG Hongyu, ZHAO Yongle, ZHANG Yongfa. Effect of secondary isothermal condensation modification on the performance of g-C₃N₄ photocatalyst[J]. Chemical Industry and Engineering Progress, 2021, 40(6): 3389-3400.

图/表 16

图1 样品CN-3h、CN-4h、CN-3h-1h、CN-3h-4h的制备示意图

图2 样品CN-3h、CN-4h、CN-3h-1h和CN-3h-4h的FTIR图

图3 样品CN-3h、CN-4h、CN-3h-1h和CN-3h-4h的XRD图

图4 样品CN-3h、CN-4h、CN-3h-1h、CN-3h-4h的氮吸附-脱附等温线（嵌入图为BJH孔隙大小分布曲线）

表1 CN-3h、CN-4h、CN-3h-1h和CN-3h-4h样品的比表面积、孔容积、平均孔径和RhB降解率

样品	比表面积 /m²·g^-1	孔容积 /mL·g^-1	平均孔径 /nm	罗丹明B降解率 /%
CN-3h	12.95	0.072	22.12	42
CN-4h	13.40	0.071	21.28	58
CN-3h-1h	15.42	0.094	24.42	71
CN-3h-4h	29.83	0.334	44.82	98

图5 不同处理条件得到的样品的SEM图

图6 样品CN-3h-4h的TEM图

图7 样品CN-3h和CN-3h-4h的SEM mapping图

图8 样品CN-3h、CN-4h、CN-3h-1h和CN-3h-4h的XPS分析谱图

表2 CN-3h、CN-4h、CN-3h-1h和CN-3h-4h催化剂表面C、N组成

样品	N元素摩尔分数 /%^①	C元素摩尔分数 /%^①	三种N拟合峰含量与总N含量比/%^②			三种C拟合峰含量与总C含量比/%^②
样品	N元素摩尔分数 /%^①	C元素摩尔分数 /%^①	C—N $? ????$ C	N—（C）₃	C—NH	N—C $? ????$ N	C—C	C—NH_x
CN-3h	48.48	32.61	77	19	10	76	22	2
CN-4h	48.68	32.31	75	16	9	77	21	2
CN-3h-1h	47.85	32.85	76	16	8	71	26	3
CN-3h-4h	47.86	32.90	78	15	7	76	22	2

表2 CN-3h、CN-4h、CN-3h-1h和CN-3h-4h催化剂表面C、N组成

样品	N元素摩尔分数 /%^①	C元素摩尔分数 /%^①	三种N拟合峰含量与总N含量比/%^②			三种C拟合峰含量与总C含量比/%^②
样品	N元素摩尔分数 /%^①	C元素摩尔分数 /%^①	C—N $? ????$ C	N—（C）₃	C—NH	N—C $? ????$ N	C—C	C—NH_x
CN-3h	48.48	32.61	77	19	10	76	22	2
CN-4h	48.68	32.31	75	16	9	77	21	2
CN-3h-1h	47.85	32.85	76	16	8	71	26	3
CN-3h-4h	47.86	32.90	78	15	7	76	22	2

图9 样品CN-3h、CN-4h、CN-3h-1h和CN-3h-4h的元素含量分析图

图10 样品CN-3h、CN-4h、CN-3h-1h及CN-3h-4h的紫外-可见漫反射光谱图和能带带隙图

图11 样品CN-3h、CN-4h、CN-3h-1h和CN-3h-4h的价带、导带位置示意图

图12 样品CN-3h、CN-4h、CN-3h-1h和CN-3h-4h的PL荧光光谱图

图13 样品CN-3h、CN-4h、CN-3h-1h、CN-3h-2h、CN-3h-3h和CN-3h-4h在可见光照射下光催化活性评价图

图14 样品CN-3h-4h的电子捕获实验中罗丹明B的降解率

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二次等温热缩聚改性对g-C₃N₄光催化剂性能的影响

Effect of secondary isothermal condensation modification on the performance of g-C₃N₄ photocatalyst

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