Page 110 - 《精细化工》2020年第3期

第 37 卷第 3 期 精 细 化 工 Vol.37, No.3
202 0 年 3 月 FINE CHEMICALS Mar. 2020

催化与分离提纯技术
苹果酸辅助水热合成 WO 及 WO -CuCrO 的
3
3
2
光催化性能

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童春杰 ，王桂 赟 1,2* ，田伟松 ，杨 欢 ，王延吉 1,2
（1. 河北工业大学 化工学院，天津 300130；2. 绿色化工与高效节能河北省重点实验室，天津 300130）
摘要：以钨酸钠或钨酸铵为原料、硝酸为酸化剂，在苹果酸辅助作用下采用水热法合成了 WO 3 ，采用 XRD、SEM
及 Raman 光谱对样品进行了表征。结果发现：苹果酸的加入、反应温度的升高及反应时间的延长都会促进单斜
相 WO 3 的形成。探讨了苹果酸辅助下，水热反应过程中 WO 3 的转化机制。测试不同条件下制得的 WO 3 与 CuCrO 2
复合后所得复合催化剂的光催化产氢活性。结果表明：水热反应时的钨源类型、苹果酸加入量、反应温度及反
应时间对 WO 3 的性能均有影响，而水热反应所得 WO 3 样品，经热处理后再与 CuCrO 2 复合，所得 WO 3 -CuCrO 2
的活性比不经热处理制得对应样品的活性大幅提高，焙烧使 WO 3 的结晶完整性得到改善。300 W 氙灯照射下，
WO 3 -CuCrO 2 光催化分解纯水 1 h 可产氢 8 μmol 以上。
关键词：WO 3 ；水热法；苹果酸；光催化；制氢；催化技术
中图分类号：O643.3 文献标识码：A 文章编号：1003-5214 (2020) 03-0528-12

Synthesis of WO 3 by hydrothermal method with malic acid and

photocatalytic performance of WO 3-CuCrO 2

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TONG Chunjie , WANG Guiyun 1,2* , TIAN Weisong , YANG Huan , WANG Yanji
（1. College of Chemical Engineering, Hebei University of Technology, Tianjin 300130, China; 2. Key Laboratory of
Green Chemicals and Energy-Efficient Hebei Province, Tianjin 300130, China）
Abstract: Tungsten oxide (WO 3) was synthesized by hydrothermal method using sodium tungstate or
ammonium tungstate as raw material, nitric acid as acid source and malic acid as assistant agent. The
samples were characterized by XRD, SEM and Raman spectroscopy. The results indicated that the addition
of malic acid, the increase of reaction temperature and the extension of reaction time were favorable for the
formation of monoclinic WO 3. The formation mechanism of monoclinic WO 3 in the malic acid-assisted
hydrothermal process was also discussed. Furthermore, the activity of compound catalysts which were
synthesized from WO 3 prepared at different conditions and CuCrO 2 in the photocatalytic water splitting was
investigated. It was found that the performance of WO 3 was affected by tungsten source type, addition
content of malic acid, reaction temperature and reaction time. For the WO 3 samples prepared by
hydrothermal reaction, the WO 3-CuCrO 2 samples which were obtained from WO 3 with heat-treatment
exhibited higher photocatalytic activity than the corresponding samples which prepared from WO 3 without
heat-treatment. Heat-treatment improved the crystallinity of WO 3. Under the irradiation of a 300 W xenon
lamp, the photocatalytic decomposition of pure water with WO 3-CuCrO 2 for 1 h, more than 8 μmol
hydrogen was produced.
Key words: WO 3; hydrothermal method; malic acid; photocatalysis; hydrogen production; catalysis
technology

收稿日期：2019-08-13; 定用日期：2019-11-05; DOI: 10.13550/j.jxhg.20190786
基金项目：国家自然科学基金（21076058）；河北省自然科学基金（B2014202004）
作者简介：童春杰（1993—），女，硕士生，E-mail：572325128@qq.com。联系人：王桂赟（1964—），女，教授，E-mail：wgy1964@hebut.edu.cn。