CN109569723A - 2,5-二-(3,5-二羧基苯基)噻吩二甲酰胺过渡金属镉配合物的光催化性能研究 - Google Patents
2,5-二-(3,5-二羧基苯基)噻吩二甲酰胺过渡金属镉配合物的光催化性能研究 Download PDFInfo
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- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
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Abstract
本发明具体涉及一种过渡金属镉有机配合物的制备及其紫外光照射下对RhB的光催化降解作用。实验结果表明，MOF1作为光催化剂可以有效的降解罗丹明B，在6h内降解罗丹明B的比率达到了85.3％，并且MOF1作为光催化剂具有良好的循环利用性和稳定性。这说明MOFs作为光催化剂在有机染料废水处理中具有潜在的应用。
Description
技术领域
本发明属于分析化学的范畴，涉及一种过渡金属镉配合物的光催化性能研究。
背景技术
随着我国综合国力的提升，化学、化工及印染等产业得以迅猛发展，在他们带来经济效益的同时所排放的废水等严重污染了环境和水资源，对生物体的生存环境和人们正常的生活造成了很大的威胁。因此，如何有效的处理这些环境污染物就显得尤为重要。
光催化技术是一种在紫外可见光等较简单的条件下将环境污染物降解为无污染的小分子物质的过程，是一种消除污染的环境友好型技术。因此，开发具有紫外和可见光响应的高催化活性和高选择性的光催化剂，并将其应用于有机污染物的光催化降解，是当前光催化技术的研究热点。
金属有机骨架(MOFs)作为一种易于功能化的新型复合材料，它具有良好的热化学稳定性、高的比表面积和光学活性等性能，是一种新型的光催化剂，在有机废水特别是染料废水的处理中具有潜在的应用价值。目前，研究人员已经对许多典型的光催化剂进行了深入的研究并将其应用于有机染料废水处理，并取得了一定的意义。鉴于此，本发明中我们选择了具有代表性的罗丹明B水溶液来作为模拟的废水，以2，5-二-(3，5-二羧基苯基)噻吩二甲酰胺(L)作为有机配体与过渡金属镉离子构筑了金属有机骨架(MOF1)，以其作为光催化剂，对RhB进行了光催化降解实验，并探究了MOF1的循环利用性和稳定性，该研究成果将为有机染料废水的处理提供了一种有效的方法。
发明内容
本发明的目的在于提供一种可降解有机染料的新型技术。通过溶解热方法，制备过渡金属镉配合物，并以其作为光催化剂，选择具有代表性的罗丹明B水溶液来作为模拟的有机染料废水，对其进行光催化降解实验。
为实现上述目的，本发明采用下述技术方案：
本发明采用溶剂热法制备了2，5-二-(3，5-二羧基苯基)噻吩二甲酰胺(L)和过渡金属镉形成的金属有机配合物，其分子式为[Cd(L)(H2O)2]·3H2O·DMF(MOF1)(L＝2，5-二-(3，5-二羧基苯基)噻吩二甲酰胺)，其具体制备过程为：
将配体L、CdCl2·5/2H2O、、DMF和H2O置于聚四氟乙烯为内衬的密封不锈钢反应釜中，密封，在85℃下反应三天，然后缓慢降至室温，过滤，干燥得无色透明块状晶体。
本发明的过渡金属镉配合物作为光催化剂降解罗丹明B的步骤为：将80mL的罗丹明B溶液置于石英烧杯中，加入20mg MOF1，在黑暗状态下搅拌40min，达到吸附-脱附平衡。然后在500W汞灯下照射反应，每隔0.5h取样一次。然后进行离心，测定样品的紫外可见吸收光谱。通过对MOF1的光催化实验研究表明，该配合物对罗丹明B具有好的降解作用，在6h内降解率达到85.3％。
附图说明
图1 Cd(L)(H2O)2]·3H2O·DMF降解罗丹明B的紫外可见光谱图；
图2不同条件下，罗丹明B的降解率图；
图3 Cd(L)(H2O)2]·3H2O·DMF降解罗丹明B的五次循环的效果图；
图4 Cd(L)(H2O)2]·3H2O·DMF经过5次循环后的PXRD图。
具体实施方式
实施例1：[Cd(L)(H2O)2]·3H2O·DMF(MOF1)的制备
将CdCl2·5/2H2O(22.8mg，0.1mmol)、配体L1(17.4mg，0.035mmol)、DMF 3mL和H2O2mL混合后，放置在以聚四氟乙烯为内衬的密封不锈钢反应釜中，密封，在85℃下反应三天，然后缓慢降至室温，得无色透明块状晶体，过滤、洗涤干燥。产率：76.7％
实施例2：MOF1的光催化性能研究
将80mL 1×10-5mol/L的罗丹明B溶液置于石英烧杯中，加入20mg MOF1，在黑暗状态下，搅拌40min，达到吸附-脱附平衡，取样一次。然后在500W汞灯照射下反应，每隔0.5h取样一次，共取样12次。取样结束后，对其进行离心，测定其紫外可见吸收光谱，如图1所示。结果表明，MOF1在6h内降解罗丹明B的比率为85.3％。
实施例3：MOF1光催化性能的对照试验
将80mL 1×10-5mol/L的罗丹明B溶液置于石英烧杯中，分别在黑暗、自然光、无催化剂条件下，每隔0.5h取样一次。将所得样品进行离心，测其紫外可见吸收光谱，不同条件下的降解率如图2所示。通过分析不同条件下RhB的降解率变化可知，催化剂和光照是RhB降解的必要条件。当加入MOF1光催化剂且在紫外光照射下6h内罗丹明B的降解率达到了85.3％。
实施例4：MOF1的稳定性和循环利用性研究。
为了验证MOF1作为光催化剂的循环利用性，我们通过过滤、洗涤的方法对MOF1进行了5次光催化循环实验。通过对比5次光催化实验过程中RhB的降解效果发现，MOF1对RhB的降解效果几乎保持一致，这说明了MOF1在5次循环实验后仍具有较好的催化活性，如图3所示。另外，我们还测定了MOF1经5次循环后的粉末XRD，如图4所示。从图中可以看出，经5次循环实验后的粉末XRD的衍射峰位置基本吻合。说明MOF1在光催化后保持了很好的稳定性。因此，MOF1具有良好的循环利用性和稳定性能，使其成了潜在的降解有机染料的光催化材料。
Claims (4)
1.一种由2，5-二-(3，5-二羧基苯基)噻吩二甲酰胺(L)和过渡金属镉盐形成的金属有机配合物[Cd(L)(H2O)2]·3H2O·DMF(MOF1)的光催化性能研究。具体的[Cd(L)(H2O)2]·3H2O·DMF合成的步骤如下：将配体L、CdCl2·5/2H2O、、DMF和H2O置于聚四氟乙烯为内衬的密封不锈钢反应釜中，密封，在85℃下反应三天，然后缓慢降至室温，过滤，干燥得无色透明块状晶体。
2.权利要求1所述的配合物，应用于有机染料罗丹明B的光催化降解。
3.权利要求2所述的[Cd(L)(H2O)2]·3H2O·DMF配合物光催化降解罗丹明B的具体步骤为：将80mL 1×10-5mol/L的罗丹明B溶液置于石英烧杯中，加入20mg所述配合物，在黑暗状态下，搅拌40min达到吸附-脱附平衡，在500W汞灯照射下反应，每隔0.5h取样一次。然后将所得样品进行离心，测其紫外可见吸收光谱。
4.按权利要求3所述的应用，[Cd(L)(H2O)2]·3H2O·DMF配合物作为光催化剂在6h内对罗丹明B的降解率达到85.3％。
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