再生纤维素/SnS<sub>2</sub>复合材料的微波辅助水热法制备及性能

doi:10.11901/1005.3093.2016.623

材料研究学报

2017, Vol. 31

Issue (8): 627-634 DOI: 10.11901/1005.3093.2016.623

研究论文

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再生纤维素/SnS₂复合材料的微波辅助水热法制备及性能

朱墨书棋¹, 林春香¹(

), 刘以凡¹, 苏巧权¹, 刘明华^1,²

1 福州大学环境与资源学院福州 350000
2 福州大学能源与环境光催化国家重点实验室福州 350000

Preparation of Composite of SnS₂/regenerated Cellulose by Microwave-assisted Synthesis and its Properties

Moshuqi ZHU¹, Chunxiang LIN¹(

), Yifan LIU¹, Qiaoquan SU¹, Minghua LIU^1,²

1 College of Environment and Resources, Fuzhou University, Fuzhou 350000, China
2 State Key Laboratory of Photocatalysis on Energy and Environment, College of Chemistry, Fuzhou University, Fuzhou 350000, China

引用本文:

朱墨书棋, 林春香, 刘以凡, 苏巧权, 刘明华. 再生纤维素/SnS₂复合材料的微波辅助水热法制备及性能[J]. 材料研究学报, 2017, 31(8): 627-634.
Moshuqi ZHU, Chunxiang LIN, Yifan LIU, Qiaoquan SU, Minghua LIU. Preparation of Composite of SnS₂/regenerated Cellulose by Microwave-assisted Synthesis and its Properties[J]. Chinese Journal of Materials Research, 2017, 31(8): 627-634.

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摘要:

分别以四氯化锡、硫代乙酰胺和再生纤维素为锡源、硫源和载体,用微波辅助加热方法在120℃制备再生纤维素/SnS₂可见光催化复合材料,使用XRD、SEM、TEM、DRS和BET等手段对其结构及性能进行了表征。结果表明,所制备的SnS₂为六方相,复合材料呈纳米薄片层状结构,晶面间距约为0.52 nm;与未负载的SnS₂相比,复合材料具有较大的可见光吸收区域及较大比表面积;用微波加热方法可降低SnS₂的合成时间和温度,在微波辐射温度为120℃、辐射时间为20~80 min的条件下制备出的再生纤维素/SnS₂复合材料在可见光照射下对20 mg/L罗丹明B的3 h内去除率可达100%,重复使用5次后对罗丹明B的可见光降解率仍可达88%。

关键词 ：复合材料, 微波辅助, SnS₂, 再生纤维素, 可见光催化

Abstract：

A visible-light catalytic composite material of regenerated cellulose supported SnS₂ (SnS₂/regenerated cellulose) was synthesized via microwave-assisted heating method at 120℃ with SnCl₄ and thioacetamide as the source of Sn and S respectively. The obtained SnS₂/regenerated cellulose was characterized by power X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-vis diffuse reflectance spectra (DRS) and specific surface areas (BET). The results show that the prepared SnS₂ is a phase with hexagonal crystal structure and the composite exhibited a nano-sized lamellar structure with 0.52 nm of interlayer spacing. In comparison with the simple SnS₂, the composite SnS₂/regenerated cellulose has larger absorption band for visible light and specific surface area. Furthermore, the microwave heating method can greatly reduce the synthesis temperature and the reaction time. The composite prepared at 120℃ for 20~80 min exhibited excellent photocatalytic performance. The removal efficiency for Rhodamine B (20 mg/L) can reach 100% within 3 h by the composite under visible light irradiation, and the degradation ratio of RhB can still reach 88% by the composite even after five cycles of use/regeneration.

Key words： composite microwave-assited SnS₂ regenerated cellulose visible-light photocatalysis

收稿日期: 2016-10-24

ZTFLH:

TB322

基金资助:国家自然科学基金(2015J01049);福建省自然科学基金(2015J01049);福州大学能源与环境光催化国家重点实验室自主课题基金(2014C02), 福建省教育厅科技项目(JZ160416)

作者简介:

作者简介朱墨书棋,女,1991年生,硕士生

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https://www.cjmr.org/CN/10.11901/1005.3093.2016.623 或 https://www.cjmr.org/CN/Y2017/V31/I8/627

图1 再生纤维素/SnS2复合材料、未负载的SnS2以及再生纤维素的XRD图谱

图2 未负载SnS2(a),再生纤维素/SnS2复合材料的电镜扫描图(b, c)及复合材料的EDS图谱(d)

图3 未负载SnS2的TEM图(a)及(a)中白色方框区域放大图(b);复合材料的TEM图(c)及(c)中白色方框区域放大图(d);(e)为复合材料的HRTEM图

图4 复合材料(a)和未负载SnS2(b)的紫外-可见漫反射谱图

图5 未负载SnS2(a)和复合材料(b)在可见光下的光电流响应曲线

图6 复合材料、未负载SnS2以及N2吸附-脱附曲线图;插图为孔径分布图

图7 不同温度影响下再生纤维素/SnS2复合光催化材料的光催化降解图(a)和XRD图(b)

图8 不同时间影响下再生纤维素/SnS2复合光催化材料的光催化降解图(a)和XRD图(b)

图9 不同纤维素添加量下再生纤维素/SnS2复合光催化材料的光催化降解图(a)和XRD图(b)

图10 未负载SnS2、纤维素和复合材料可见灯下的光催化材料的光催化降解性能

图11 复合材料回收使用次数对罗丹明B光催化脱色效率的影响

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