CN108176409B - 一种氢钨青铜/硫化镉复合光催化剂的制备方法 - Google Patents
一种氢钨青铜/硫化镉复合光催化剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种氢钨青铜/硫化镉复合光催化剂的制备方法，其以WCl6作为前驱物，正丙醇为溶剂，经溶剂热反应生成W18O49；然后加入乙酸镉和硫脲，经水浴反应生成W18O49/CdS；再将其经原位光诱导还原，制得所述复合光催化剂H0.53WO3/CdS。本发明制备方法新颖、操作简单方便、合成高效、成本低，且其首次将氧化钨光致变色现象的激发光拓展至可见光，并与光催化过程相结合，利用氢钨青铜快速传递电子且吸光能力强等优势，不仅有效提高了复合光催化剂光生载流子的分离，降低了载流子的复合率，还大大提高了复合光催化剂的吸光能力，使其表现出优异的光催化产氢性能，而在探索清洁可再生能源领域具有广阔的应用前景。
Description
技术领域
本发明属于光催化领域，具体涉及一种氢钨青铜/硫化镉新型复合光催化剂的制备方法及所得复合光催化剂在光解水产氢中的应用。
背景技术
钨青铜是稳定性较高的具有深蓝色金属光泽的阳离子掺杂金属氧化物，一般用MxWO3表示，呈现出金属导体或者半导体的性质，其颜色与性能随着M与x的不同会产生相应的差异。钨青铜型材料在铁电、压电、热释电、非线性光学等方面具有独特而优异的性能，从而逐渐得到广泛的关注，目前在电子材料研究领域里已经成为仅次于钙钛矿型材料的第二大类电子材料团，然而，有关其在光催化领域应用的报道还比较少。
目前已有一些制备纳米钨青铜的报道，如专利CN 103496744A公开了一种还原态铵钨青铜的合成方法，其使用WCl6作为钨源，加入油酸作为溶剂，W：NH4 +的摩尔比为1：（0.2～ 0.3），在150～350 ℃的高温条件下晶化反应0 .5～48 h，最终获得还原态铵钨青铜纳米粉体。这种方法合成时间长、产率低、成本高，且所得产物红外吸收性能较差。而专利CN104528829A报道了使用钨酸盐溶液通过阳离子交换得到钨酸溶胶，再加入还原剂与铯源得到相应的前驱体，将前驱体加入到反应釜中进行水热反应后可制得铯钨青铜纳米盐。该方法在制备前躯体的过程中使用了阳离子交换法，因此单次合成的量有限，且水热合成法耗时较长，反应过程中需要高温高压条件，能耗较大，对设备的要求较高。因此，纳米钨青铜特别是氢钨青铜的工业化合成已成为制约其广泛应用的瓶颈。
CdS作为一种重要的可见光催化剂，具有独特的电学、光学、磁学及发光性能，在光催化反应中得到广泛的研究。但单一的CdS内光生电荷的传输和分离效率较低，电子和空穴对的体相复合严重，从而大大降低了材料的光催化性能。目前，针对CdS的上述缺点开展了很多研究，例如将助催化剂与CdS复合，达到提高光催化活性的目的。目前用于构造CdS复合光催化剂的助催化剂主要包括一些贵金属、石墨烯以及过渡金属硫属化物，而关于将钨青铜作为助催化剂与CdS组合用于可见光下分解水制氢还未见公开报道。
发明内容
本发明的目的在于提供一种氢钨青铜/硫化镉复合光催化剂的制备方法，其采用W18O49和CdS的复合物作为前驱体，在乳酸的作用下利用硫化镉与W18O49良好的能带匹配度，经过可见光照射快速得到H0.53WO3/CdS复合物，具有制备工艺要求低、操作方便、合成高效的特点，且所得H0.53WO3/CdS复合物具有高效的光催化产氢效果。
为实现上述目的，本发明采用如下技术方案：
一种氢钨青铜/硫化镉复合光催化剂的制备方法，其包括以下步骤：
（1）以WCl6作为前驱物，正丙醇为溶剂，于120-220℃溶剂热反应20-30h，得到W18O49；
（2）将步骤（1）得到的W18O49分散于水中，并加入乙酸镉和硫脲，65-90℃水浴反应0.5-3h，得到W18O49/CdS；其中，乙酸镉和硫脲的质量比为1-2:1，所得W18O49/CdS中W18O49与CdS质量比为1:20-1:30；
（3）将步骤（2）得到的W18O49/CdS加入到体积比5:1-20:1的水和乳酸的混合溶液中，于太阳光或人工光源下照射0.5-2h得到所述复合光催化剂H0.53WO3/CdS。
本发明制备工艺要求低、操作方便、合成高效，其所得H0.53WO3/CdS复合物具有高效的光催化产氢效果。
附图说明
图1为实施例1所得W18O49/CdS和H0.53WO3/CdS的X射线衍射图谱。
图2为实施例1所得H0.53WO3/CdS在牺牲剂存在条件下光解水产氢的情况。从图2可以看出，本发明H0.53WO3/CdS复合物在同等条件下的产氢量远高于未复合的CdS，且随着光照时间的延长，H0.53WO3/CdS复合物的产氢量迅速提高。
具体实施方式
为了使本发明所述的内容更加便于理解，下面结合具体实施方式对本发明所述的技术方案做进一步的说明，但是本发明不仅限于此。
实施例1
称取200mg WCl6，加入到50mL正丙醇中，于120℃保温反应24小时，经乙醇和水洗涤，干燥后，得到W18O49；称取所得W18O49 40mg，分散于60mL H2O中，加入1.48g乙酸镉和0.8g硫脲，于80℃水浴保温反应30分钟，得到W18O49/CdS；取200mgW18O49/CdS，加入90mL水和10mL乳酸组成的混合溶液中，然后光照1h，得到H0.53WO3/CdS复合物。
实施例2
称取200mg WCl6，加入到50mL正丙醇中，于180℃保温反应20小时，经乙醇和水洗涤，干燥后，得到W18O49；称取所得W18O49 80mg，分散于60mL H2O中，加入1.48g乙酸镉和0.8g硫脲，于85℃水浴保温反应60分钟，得到W18O49/CdS；取300mgW18O49/CdS，加入90mL水和10mL乳酸组成的混合溶液中，然后光照0.5h，得到H0.53WO3/CdS复合物。
实施例3
称取200mg WCl6，加入到50mL正丙醇中，于200℃保温反应20小时，经乙醇和水洗涤，干燥后，得到W18O49；称取所得W18O49 60mg，分散于80mL H2O中，加入2.96g乙酸镉和1.6g硫脲，于85℃水浴保温反应30分钟，得到W18O49/CdS；取500mgW18O49/CdS，加入90mL水和10mL乳酸组成的混合溶液中，然后光照0.5h，得到H0.53WO3/CdS复合物。
以上所述仅为本发明的较佳实施例，凡依本发明申请专利范围所做的均等变化与修饰，皆应属本发明的涵盖范围。
Claims (5)
1.一种氢钨青铜/硫化镉复合光催化剂的制备方法，其特征在于：包括以下步骤：
（1）以WCl6作为前驱物，正丙醇为溶剂，通过溶剂热反应得到W18O49；
（2）将步骤（1）得到的W18O49分散于水中，并加入乙酸镉和硫脲，水浴反应得到W18O49/CdS；
（3）将步骤（2）得到的W18O49/CdS加入到水和乳酸的混合溶液中，经光照得到所述复合光催化剂H0.53WO3/CdS。
2.根据权利要求1所述的制备方法，其特征在于：步骤（1）中所述溶剂热反应的温度为120-220℃，时间为20-30h。
3.根据权利要求1所述的制备方法，其特征在于：步骤（2）中乙酸镉和硫脲的质量比为1-2:1；
所述水浴反应的温度为65-90℃，时间为0.5-3h；
所得W18O49/CdS中W18O49与CdS质量比为1:20-1:30。
4.根据权利要求1所述的制备方法，其特征在于：步骤（3）所述混合溶液中水和乳酸的体积比为5:1-20:1；
所述光照是于太阳光或人工光源下照射0.5-2h。
5.一种如权利要求1所述方法制得的氢钨青铜/硫化镉复合光催化剂在光解水产氢中的应用。
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810049771.8A CN108176409B (zh) | 2018-01-18 | 2018-01-18 | 一种氢钨青铜/硫化镉复合光催化剂的制备方法 |
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| CN104528829A (zh) * | 2014-12-23 | 2015-04-22 | 深圳市嘉达高科产业发展有限公司 | 铯钨青铜粉体的制备方法和功能膜 |
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| CN104528829A (zh) * | 2014-12-23 | 2015-04-22 | 深圳市嘉达高科产业发展有限公司 | 铯钨青铜粉体的制备方法和功能膜 |
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| Direct Z-scheme composite of CdS and oxygen-defected CdWO4: An efficient visible-light-driven photocatalyst for hydrogen evolution;Xu Jia et al.;《Applied Catalysis B: Environmental》;20160521;第198卷;第154-161页 |
| Enhancement of Photocatalytic H2 Evolution on CdS by Loading MoS2 as Cocatalyst under Visible Light Irradiation;Xu Zong, et al.;《J. AM. CHEM. SOC.》;20080513;第130卷;第7176–7177页 |
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