CN112058279B - 一种光催化降解有机污水制氢催化剂的制备及应用方法 - Google Patents
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Abstract
本发明属于光催化技术领域，本发明公开了一种光催化降解有机污水制氢催化剂的制备及应用方法，应用于降解有机废水同时制取氢气，表现为利用太阳能处理废水并获取绿色、可储备的氢能，呈现出“变废为宝”应用价值。具体地，通过化学共溶法制备的纳米粉末光催化剂为表面共轭亚硫酸根基团的硫化镉纳米颗粒(CdS@SO3)，在太阳光的激发下生成活性的电子和空穴，其中光生导带电子能够还原水中质子生成氢气，同时表面亚硫酸根(‑SO3)基团作为电子传输桥梁从吸附的有机分子中俘获电子填充价态空穴，有机分子被氧化分解，实现电荷氧化‑还原反应循环，且光催化剂本身保持稳定。
Description
技术领域
本发明涉及一种光催化降解有机污水制氢催化剂的制备及应用方法，属于纳米能源功能材料领域。
背景技术
长期以来，化石燃料的大规模使用，导致了日益严重的环境污染和能源危机，发展清洁、可再生能源是人类社会可持续发展的必要任务之一。氢气具有能量密度高、可存储移动、便于重整转化、燃烧无污染等一系列优点，被认为是理想的绿色能源载体。基于半导体光催化技术，将清洁、丰富的太阳能转化为氢气燃料，被誉为“人工光合作用”，在科学界得到了广泛的研究。其中，硫化镉（CdS）是一个典型的半导体光催化剂，具有合适的能带结构确保太阳光吸收和还原反应动力，在光催化还原水质子制氢应用中备受关注。然而, 较低的光生电荷分离效率严重限制着CdS催化剂的实际应用。本专利在CdS纳米颗粒表面共轭组装亚硫酸根（-SO3）基团，用于快速俘获光生空穴，促进电子-空穴对的分离利用效率。因此，CdS@SO3催化剂在太阳光辐照下催化有机尿素废水生成氢气（2H++2e-→H2），同时尿素被氧化降解（CO(NH2)2 + 6OH- + 6h+ → N2 + CO2 + 5H2O），展现了“变废为宝”的应用策略。
发明内容
本发明的目的在于提供一种光催化降解有机污水制氢催化剂的制备及应用方法。
实现本发明目的的技术解决方案是：
本发明提供一种光催化降解有机污水制氢催化剂的制备方法。
该催化剂为表面包裹-SO3基团的CdS纳米颗粒催化剂，采用化学共溶法制备，步骤如下：
首先，分别配置Cd(CH3CO2)2和Na2S水溶液；
然后，将Cd(CH3CO2)2溶液逐滴滴入Na2S水溶液，并伴随着磁力搅拌；滴入完成后，超声混合溶液，促进样品成核和分散性；
最后，使用高速离心分离样品，并用去离子水和乙醇反复清洗样品，去除残留或吸附离子，经过60℃的干燥获得粉末样品。
最佳的，预配置的Cd(CH3CO2)2和Na2S的溶液的浓度分别为7.5g/L 和0.1g/mL。
最佳的，按体积比为1:20，将少量的Cd(CH3CO2)2溶液滴入Na2S溶液。
最佳的，混合溶液中Cd2+和S2-离子的摩尔比约在1:910。
最佳的，混合溶液通过超声10min，促进结晶成核和颗粒分散。
最佳的，通过每分钟12000转的高速离心分离并清洗纳米颗粒样品。
最佳的，通过60℃下干燥获得粉末样品。
上述纳米催化剂在光催化降解有机污水制氢的应用，直接将制备的纳米颗粒催化剂按0.1g/L的剂量加入到20g/L的尿素水溶液中，用带有AM1.5滤片的氙灯模拟太阳光辐照，光强为100mW/cm-2。反应器密封连接到气相色谱，跟踪探测光催化反应的生成氢气和氮气，演示光催化降解尿素废水生产氢气的应用价值。
与现有光催化剂相比，本发明相对于现有技术相比具有显著优点：1、制备原料廉价、工艺简单，可工业化拓展，具有成本优势；2、可见光波段响应，氢气演化活性高，不需要额外的牺牲剂；3、同时催化降解有机废水，变废为宝实现双效益。
附图说明
图1是本发明公开的纳米催化剂的X射线衍射图谱。
图2是本发明公开的纳米催化剂的透射电子显微镜照片。
图3是本发明公开的纳米催化剂的傅里叶红外光谱。
图4是本发明公开的纳米催化剂的光催化尿素废水氢气演化的氢气演化时程图。
图5是本发明公开的纳米催化剂的光催化尿素废水氮气演化的氢气演化时程图。
图6是本发明公开的纳米催化剂使用不同剂量时演化氢气速率比较的氢气演化速率图。
图7是本发明公开的纳米催化剂在不同浓度尿素废水中演化氢气速率比较的氢气演化速率图。
实施方式
下面结合附图及实施例对本发明做进一步说明
本发明公开一种光催化降解有机污水制氢催化剂的制备与应用方法，具体实施过程，包括：（1）化学共溶法制备表面包裹亚硫酸根基团的硫化镉纳米颗粒催化剂；（2）纳米催化剂应用于太阳光降解有机尿素废水，同时制取氢气，展现“变废为宝”的应用价值。
实施例
催化剂的制备：首先，分别配置7.5g/L的Cd(CH3CO2)2水溶液和0.1g/mL的Na2S水溶液；然后，按1:20的体积比，将Cd(CH3CO2)2溶液逐滴加入Na2S水溶液，并伴随着磁力搅拌；滴入完成后，混合溶液超声10min，促进样品成核和分散性；最后，使用每分钟12000转的高速离心分离样品，并用去离子水和乙醇反复清洗样品，去除残留或吸附离子，经过60℃的干燥获得黄绿色粉末样品。
催化剂的结构表征：首先，通过X射线衍射仪（XRD）对制得的样品进行微结构分析，如图1所示，样品的XRD图谱显示立方相CdS特征衍射峰，证实了样品的结晶。然后，利用透射电子显微镜（TEM）观察样品形貌，如图2所示，样品呈现为5-10nm大小的纳米颗粒，用傅里叶变换红外（FTIR）光谱揭示颗粒表面含有丰富亚硫酸基团。
催化剂的应用方法：将制备的纳米颗粒催化剂按0.1g/L的剂量加入到20g/L的尿素水溶液中，用带有AM1.5滤片的氙灯模拟太阳光辐照，光强为100mW/cm-2。反应器密封连接到气相色谱，跟踪探测光催化反应的生成气体：氢气和氢气，演示了光催化降解尿素废水生产氢气的应用价值。如图4和5所示，氢气和氮气生成量几乎随着光催化反应时间呈线性关系，说明光催化反应的稳定性，而且催化剂在多次反复使用循环实验中活性没有明显衰减。
对比例1
改变纳米颗粒催化剂的使用剂量分别为0.05g/L、0.1g/L、0.15g/L、0.3g/L和0.5g/L，保持其它实验条件不变（20g/L的尿素水溶液；AM1.5滤片模拟太阳光辐照，光强为100mW/cm-2），依次进行光催化测试，链接反应器的气相色谱跟踪探测反应生成气体。如图6所示，催化剂使用剂量为0.1g/L时，氢气演化速率最快，选定为最优催化剂剂量。
对比例2
在催化剂保持0.1g/L的最优剂量下，改变尿素水溶液的浓度分别为5g/L、10g/L、15g/L和20g/L，其它实验条件不变（AM1.5滤片模拟太阳光辐照，光强为100mW/cm-2），依次进行光催化性能测试，链接反应器的气相色谱跟踪探测反应生成气体。如图7所示，尿素溶液的浓度为20g/L时，氢气演化速率最快，选定为反应液的最佳浓度。
对比例3
使用表面无修饰的商用高纯CdS纳米颗粒作为对照催化剂，保持其它实验条件（0.1g/L的催化剂用量；20g/L的尿素水溶液；带有AM1.5滤片的氙灯模拟太阳光辐照，光强为100mW/cm-2）完全一致，进行光催化测试。气相色谱跟踪探测光催化产物，并没有检测到任何的气体生成。原因是CdS纳米颗粒本身是非常的荧光半导体材料，超快的光激子复合和对应的高荧光效率使得光生电荷没有机会迁移至表面参与较慢的催化反应。
因此，本发明优势主要体现为：1、表面修饰-SO3基团，作为空穴传输链，促进电荷分离动力；2、用尿素氧化反应取代水氧化反应，不仅降低全反应热力学势垒，而且克服了CdS基催化剂通常存在的光阳极腐蚀问题。
总之，本发明的CdS@SO3纳米催化剂在太阳光辐照下催化有机尿素废水生成氢气（2H++2e-→H2），同时尿素被氧化降解（CO(NH2)2 + 6OH- + 6h+ → N2 + CO2 + 5H2O），展现了“变废为宝”的应用价值，为推进太阳能转化为可储备的化学能提供了一种廉价、可行的策略。
Claims (5)
1.一种光催化降解有机污水制氢催化剂的应用方法，其特征在于，化学共溶法制备表面包裹亚硫酸根-SO3基团的硫化镉CdS纳米颗粒催化剂，该催化剂为表面包裹-SO3基团的CdS纳米颗粒催化剂，采用化学共溶法制备，步骤如下：
首先，分别配置Cd(CH3CO2)2和Na2S水溶液；
然后，将Cd(CH3CO2)2溶液逐滴滴入Na2S水溶液，并伴随着磁力搅拌；滴入完成后，超声混合溶液，促进样品成核和分散性；
最后，使用高速离心分离样品，并用去离子水和乙醇反复清洗样品，去除残留或吸附离子，经过60℃的干燥获得粉末样品；
混合溶液中Cd2+和S2-离子的摩尔比在1:910；
光催化降解有机污水制氢应用具体过程包括：直接将制备的纳米颗粒催化剂按0.1g/L的剂量加入到20g/L的尿素水溶液中，用带有AM1.5滤片的氙灯模拟太阳光辐照，光强为100mW/cm-2；反应器密封连接到气相色谱，跟踪探测光催化反应的生成气体为氢气和氮气。
2.根据权利要求1所述的光催化降解有机污水制氢催化剂的应用方法，其特征在于，所述催化剂为表面包裹-SO3基团的CdS纳米颗粒，颗粒大小为7~10nm。
3.根据权利要求1所述的光催化降解有机污水制氢催化剂的应用方法，其特征在于，预配置的Cd(CH3CO2)2和Na2S的溶液的浓度分别为7.5g/L 和0.1g/mL。
4.根据权利要求1所述的光催化降解有机污水制氢催化剂的应用方法，其特征在于，按体积比为1:20，将少量的Cd(CH3CO2)2溶液滴入Na2S溶液。
5.根据权利要求1所述的光催化降解有机污水制氢催化剂的应用方法，其特征在于，混合溶液通过超声10min，促进结晶成核和颗粒分散；通过12000转每分的高速离心分离并清洗纳米颗粒样品。
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