CN107233899A - 一种CdS量子点/Bi2MoO6/石墨烯复合型光催化剂的制备方法 - Google Patents
一种CdS量子点/Bi2MoO6/石墨烯复合型光催化剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种CdS量子点/Bi2MoO6/石墨烯复合型光催化剂的制备方法，属于无机环保光催化材料的合成技术领域。本发明的技术方案要点为：一种CdS量子点/Bi2MoO6/石墨烯复合型光催化剂的制备方法，是由CdS量子点、Bi2MoO6和石墨烯复合而形成的CdS量子点/Bi2MoO6/石墨烯复合型光催化剂，其中CdS量子点和Bi2MoO6的摩尔比为1:0.1‑0.5，石墨烯与Bi2MoO6的质量比为0.03‑0.15:1。本发明制得的CdS量子点/Bi2MoO6/石墨烯复合型光催化剂有效减少光生电子和空穴的复合速率，提高了CdS量子点的光解水制氢催化活性并减缓了CdS量子点在光解水过程中光蚀现象的发生，具有操作条件温和、所制备的产品团聚程度低及光催化活性高的优点。
Description
技术领域
本发明属于无机环保光催化材料的合成技术领域，具体涉及一种CdS量子点/Bi2MoO6/石墨烯复合型光催化剂的制备方法。
背景技术
氢能作为一种高效清洁的绿色化学能源，对于解决全球愈发紧张的能源和环境危机有着重要的意义。近几十年来，研究者们一直致力于光解水制氢技术的研究，开发了许多具有制氢性能的光催化材料。在众多的光催化材料中，CdS量子点作为一种典型的半导体纳米材料，具有较窄的禁带宽度、较好的光利用率及适宜的导带电势，在光催化产氢研究中表现出巨大的应用潜力。然而在实际应用中，CdS量子点存在的光腐蚀现象严重，同时由于光生载流子高的复合率，导致其光催化制氢量子效率偏低。
为了克服CdS量子点光催化剂在制氢过程中的缺陷，学者们对其做大量的改性研究，发现材料复合能有效的阻止CdS量子点光蚀现象的发生和明显提高其制氢量子效率。钼酸铋（Bi2MoO6）是一种典型的铋系光催化剂，具有可见光光催化性能。如将CdS量子点与具有合适带隙结构的Bi2MoO6相复合，利用两种半导体的能级差使光生载流子在两者的导带和价带之间互相迁移，促进光生电子和空穴的分离，进而提高其光分解水制氢的催化性能。此外，石墨烯是新型二维碳纳米材料，具有更大的比表面积、高化学稳定性及更为优异的电子传导性能。如将石墨烯与CdS量子点复合，利用石墨烯规整的二维平面结构作为光催化剂的载体，一方面可以提高CdS量子点的分散程度，增加反应活性位；另一方面可加快光生电荷迁移的速率，提高CdS量子点的光催化活性并防止光蚀现象的发生。
发明内容
本发明解决的技术问题是提供了一种操作简单且易于实现的CdS量子点/Bi2MoO6/石墨烯复合型光催化剂的制备方法，该方法制得的CdS量子点/Bi2MoO6/石墨烯复合型光催化剂可见光利用率高、光蚀现象低且光催化制氢活性好。
本发明为解决上述技术问题采用如下技术方案，一种CdS量子点/Bi2MoO6/石墨烯复合型光催化剂的制备方法，其特征在于具体步骤为：
（1）在搅拌条件下将五水合硝酸铋和二水合钼酸钠按摩尔比2:1溶于去离子水中形成硝酸铋与钼酸钠的混合溶液，在室温条件下将硝酸铋与钼酸钠的混合溶液搅拌2h后转移至水热反应釜中，然后将水热反应釜放入微波消解仪中于120℃微波反应5-30min，待反应结束后冷却、洗涤、干燥得到Bi2MoO6纳米粉体；
（2）配制乙酸镉溶液，在搅拌和通氮气的情况下向乙酸镉溶液中加入巯基乙酸和硫化钠得到混合溶液，其中巯基乙酸与乙酸镉的摩尔比为1.2:1，硫化钠与乙酸镉的摩尔比为1:1；
（3）将步骤（2）得到的混合溶液于65℃反应2h，然后加入石墨烯和步骤（1）得到的Bi2MoO6纳米粉体得到悬浮溶液，其中石墨烯与Bi2MoO6纳米粉体的质量比为0.03-0.15:1，Bi2MoO6纳米粉体与乙酸镉的摩尔比为0.1-0.5:1；
（4）将步骤（3）得到的悬浮溶液继续反应0.5h后过滤、干燥得到具有高催化活性的CdS量子点/Bi2MoO6/石墨烯复合型光催化剂。
进一步优选，所述硝酸铋与钼酸钠的混合溶液中硝酸铋的摩尔浓度为0.01-0.05mol/L。
进一步优选，所述乙酸镉溶液中乙酸镉的摩尔浓度为0.01-0.05mol/L。
本发明与现有技术相比具有以下有益效果：
1、采用适宜的合成工艺制备出能带结构相匹配的CdS量子点/Bi2MoO6/石墨烯复合型光催化剂，利用两种半导体之间的能级差使光生载流子由一种半导体微粒的能级注入到另一种半导体微粒的能级上，从而提高光生电荷的分离效率，进而提高复合型光催化剂的制氢性能；
2、利用石墨烯优异的电子传导性能，不但提高了CdS量子点光催化剂的制氢效率，同时也有效降低了CdS量子点的光蚀性能；
3、根据微波水热法加热速率快和溶液受热均匀等特点，采用微波水热法制备出晶粒粒度小、团聚程度低的高活性Bi2MoO6纳米粉体，进而有效提高了CdS量子点/Bi2MoO6/石墨烯复合型光催化剂的活性。
附图说明
图1为300W氙灯照射下，本发明实施例1所制备的CdS量子点/Bi2MoO6/石墨烯复合型光催化剂和纯CdS量子点光催化剂的光催化分解水制氢效率柱形图（操作条件：催化剂的量：0.1g；牺牲剂的量：5mL 0.1mol/L的Na2S和5mL 0.04mol/L的Na2SO3）。从图中可以看出，在模拟可见光的照射下，光照5h后，CdS量子点/Bi2MoO6/石墨烯复合型光催化剂的产氢效率明显高于纯CdS量子点光催化剂的产氢效率，表现出明显增强的光催化活性。
具体实施方式
以下通过实施例对本发明的上述内容做进一步详细说明，但不应该将此理解为本发明上述主题的范围仅限于以下的实施例，凡基于本发明上述内容实现的技术均属于本发明的范围。
实施例1
（1）在搅拌条件下将0.97g五水合硝酸铋和0.242g二水合钼酸钠溶于200mL去离子水中形成硝酸铋与钼酸钠的混合溶液，在室温条件下将硝酸铋与钼酸钠的混合溶液搅拌2h后转移至水热反应釜中，然后将水热反应釜放入微波消解仪中于120℃微波反应5min，待反应结束后冷却、洗涤、干燥得到Bi2MoO6纳米粉体；
（2）配制0.01mol/L的乙酸镉溶液200mL，在搅拌和通氮气的情况下向乙酸镉溶液中加入0.0024mol巯基乙酸和0.002mol硫化钠得到混合溶液；
（3）将步骤（2）得到的混合溶液于65℃反应2h，然后加入0.135g石墨烯和0.001mol步骤（1）得到的Bi2MoO6纳米粉体得到悬浮溶液；
（4）将步骤（3）得到的悬浮溶液继续反应0.5h后过滤、干燥得到具有高催化活性的CdS量子点/Bi2MoO6/石墨烯复合型光催化剂。
实施例2
（1）在搅拌条件下将1.94g五水合硝酸铋和0.484g二水合钼酸钠溶于200mL去离子水中形成硝酸铋与钼酸钠的混合溶液，在室温条件下将硝酸铋与钼酸钠的混合溶液搅拌2h后转移至水热反应釜中，然后将水热反应釜放入微波消解仪中于120℃微波反应10min，待反应结束后冷却、洗涤、干燥得到Bi2MoO6纳米粉体；
（2）配制0.03mol/L的乙酸镉溶液200mL，在搅拌和通氮气的情况下向乙酸镉溶液中加入0.0072mol巯基乙酸和0.006mol硫化钠得到混合溶液；
（3）将步骤（2）得到的混合溶液于65℃反应2h，然后加入0.135g石墨烯和0.002mol步骤（1）得到的Bi2MoO6纳米粉体得到悬浮溶液；
（4）将步骤（3）得到的悬浮溶液继续反应0.5h后过滤、干燥得到具有高催化活性的CdS量子点/Bi2MoO6/石墨烯复合型光催化剂。
实施例3
（1）在搅拌条件下将0.97g五水合硝酸铋和0.242g二水合钼酸钠溶于200mL去离子水中形成硝酸铋与钼酸钠的混合溶液，在室温条件下将硝酸铋与钼酸钠的混合溶液搅拌2h后转移至水热反应釜中，然后将水热反应釜放入微波消解仪中于120℃微波反应30min，待反应结束后冷却、洗涤、干燥得到Bi2MoO6纳米粉体；
（2）配制0.05mol/L的乙酸镉溶液200mL，在搅拌和通氮气的情况下向乙酸镉溶液中加入0.012mol巯基乙酸和0.01mol硫化钠得到混合溶液；
（3）将步骤（2）得到的混合溶液于65℃反应2h，然后加入0.1g石墨烯和0.001mol步骤（1）得到的Bi2MoO6纳米粉体得到悬浮溶液；
（4）将步骤（3）得到的悬浮溶液继续反应0.5h后过滤、干燥得到具有高催化活性的CdS量子点/Bi2MoO6/石墨烯复合型光催化剂。
实施例4
（1）在搅拌条件下将4.85g五水合硝酸铋和1.21g二水合钼酸钠溶于200mL去离子水中形成硝酸铋与钼酸钠的混合溶液，在室温条件下将硝酸铋与钼酸钠的混合溶液搅拌2h后转移至水热反应釜中，然后将水热反应釜放入微波消解仪中于120℃微波反应15min，待反应结束后冷却、洗涤、干燥得到Bi2MoO6纳米粉体；
（2）配制0.05mol/L的乙酸镉溶液200mL，在搅拌和通氮气的情况下向乙酸镉溶液中加入0.012mol巯基乙酸和0.01mol硫化钠得到混合溶液；
（3）将步骤（2）得到的混合溶液于65℃反应2h，然后加入0.135g石墨烯和0.005mol步骤（1）得到的Bi2MoO6纳米粉体得到悬浮溶液；
（4）将步骤（3）得到的悬浮溶液继续反应0.5h后过滤、干燥得到具有高催化活性的CdS量子点/Bi2MoO6/石墨烯复合型光催化剂。
以上实施例描述了本发明的基本原理、主要特征及优点，本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明原理的范围下，本发明还会有各种变化和改进，这些变化和改进均落入本发明保护的范围内。
Claims (3)
1.一种CdS量子点/Bi2MoO6/石墨烯复合型光催化剂的制备方法，其特征在于具体步骤为：
（1）在搅拌条件下将五水合硝酸铋和二水合钼酸钠按摩尔比2:1溶于去离子水中形成硝酸铋与钼酸钠的混合溶液，在室温条件下将硝酸铋与钼酸钠的混合溶液搅拌2h后转移至水热反应釜中，然后将水热反应釜放入微波消解仪中于120℃微波反应5-30min，待反应结束后冷却、洗涤、干燥得到Bi2MoO6纳米粉体；
（2）配制乙酸镉溶液，在搅拌和通氮气的情况下向乙酸镉溶液中加入巯基乙酸和硫化钠得到混合溶液，其中巯基乙酸与乙酸镉的摩尔比为1.2:1，硫化钠与乙酸镉的摩尔比为1:1；
（3）将步骤（2）得到的混合溶液于65℃反应2h，然后加入石墨烯和步骤（1）得到的Bi2MoO6纳米粉体得到悬浮溶液，其中石墨烯与Bi2MoO6纳米粉体的质量比为0.03-0.15:1，Bi2MoO6纳米粉体与乙酸镉的摩尔比为0.1-0.5:1；
（4）将步骤（3）得到的悬浮溶液继续反应0.5h后过滤、干燥得到具有高催化活性的CdS量子点/Bi2MoO6/石墨烯复合型光催化剂。
2.根据权利要求1所述的CdS量子点/Bi2MoO6/石墨烯复合型光催化剂的制备方法，其特征在于：所述硝酸铋与钼酸钠的混合溶液中硝酸铋的摩尔浓度为0.01-0.05mol/L。
3.根据权利要求1所述的CdS量子点/Bi2MoO6/石墨烯复合型光催化剂的制备方法，其特征在于：所述乙酸镉溶液中乙酸镉的摩尔浓度为0.01-0.05mol/L。
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