CN108579813A - 一种在可见光驱动下具有催化活性的复合光催化剂及其制备方法和应用 - Google Patents
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Abstract
本发明涉及一种在可见光驱动下具有催化活性的复合光催化剂及其制备方法和应用。采用的技术方案是：将含有羧基的维生素B12衍生物和光敏剂RhB溶于甲醇溶液中，加入适量的TiO2(P25)纳米球，超声分散，室温搅拌，离心，产物用去离子水反复洗涤至上清液无色，真空干燥获得目标产物。本发明制备的复合光催化剂B12‑TiO2‑RhB在可见光驱动下可高效降解有机卤代物。
Description
技术领域
本发明属于催化剂材料领域，尤其涉及一种在可见光驱动下具有催化活性的复合光催化剂及其制备方法和应用。
背景技术
卤代有机污染物的大量使用和排放及残留在土壤中的有机卤代农药对环境造成的污染一直是亟待解决的问题。高效利用太阳光实现可见光催化有机卤代物降解既节省能源、又环境友好，是目前科学研究领域的热点课题之一。将脱卤催化剂、可见光光敏剂同时固载到合适的载体上，获得复合型催化剂，利用三者的协同作用有效提高催化体系对太阳光的利用率，进而提高催化效率，是构筑高效、绿色催化体系的有效方法之一。
发明内容
本发明提供了一种在可见光驱动下具有催化活性的复合光催化剂B12-TiO2-RhB。利用含有羧基的维生素B12衍生物及罗丹明B(RhB)结构中的羧基同时固载到TiO2纳米球表面上，制备出复合光催化剂B12-TiO2-RhB，该复合光催化剂在可见光驱动下催化降解有机卤代物具有广泛的应用前景。
为实现上述目的，本发明采用的技术方案是：一种在可见光驱动下具有催化活性的复合光催化剂，所述的复合光催化剂是B12-TiO2-RhB。
一种在可见光驱动下具有催化活性的复合光催化剂的制备方法，包括如下步骤：将适量的含有羧基的维生素B12衍生物和光敏剂RhB溶于甲醇溶液中，加入适量的TiO2纳米球，超声分散，常温搅拌，离心，产物用去离子水洗涤至无色，真空干燥，得目标产物。
优选的，按质量比，含有羧基的维生素B12衍生物:光敏剂RhB:TiO2＝3:1:30。
优选的，所述的含有羧基的维生素B12衍生物为[(CN)(H2O)Cob(III)7COOH]Cl。
优选的，所述的TiO2纳米球为P25型的TiO2。
上述的在可见光驱动下具有催化活性的复合光催化剂在可见光驱动下降解有机卤代物中的应用。方法如下：常温下，将上述的复合光催化剂B12-TiO2-RhB，超声分散于含有有机卤代物的甲醇溶液中，再加三乙醇胺，超声分散，反应液通入氮气除氧，并在氮气保护下可见光照射反应。更优选的，所述的有机卤代物是2,2-双(4-氯苯基)-1,1,1-三氯乙烷(DDT)。
本发明的有益效果是：
本发明中，罗丹明B(Rhodamine B，RhB)是一种鲜桃红色染料，廉价易得，在440～600nm间有较强的可见光吸收，且具有良好的氧化还原活性。维生素B12及其衍生物具有丰富的氧化还原性质和配位化学性质，可以作为催化剂用于光或电催化脱卤反应、扩环反应、分子重排、分子间甲基转移反应和核苷酸生成脱氧核苷酸等反应中。P25型二氧化钛粒径均一、催化性能高、化学性质稳定、价格低廉、热稳定性高。本发明将光敏剂罗丹明B和维生素B12催化剂引入到P25型二氧化钛表面，制备了一种绿色、廉价、易得、性能良好的复合型催化剂，该复合催化剂在可见光驱动下可实现高效催化降解有机卤代物，并且该催化剂具有良好的稳定性可实现回收再利用，具有较好的应用前景。
附图说明
图1是复合光催化剂B12-TiO2-RhB的合成路线图。
图2是维生素B12衍生物[(CN)(H2O)Cob(III)7COOH]Cl的结构示意图。
图3是罗丹明B(RhB)的结构示意图。
图4是P25型TiO2和B12-TiO2-RhB的X-射线粉末衍射图。
图5是P25型TiO2和B12-TiO2-RhB的甲醇分散液在室温下静置1h的照片。
图6是B12-TiO2-RhB可见光驱动下催化降解DDT的反应式。
具体实施方式
实施例1一种在可见光驱动下具有催化活性的复合光催化剂B12-TiO2-RhB
(一)制备方法如下：
取P25型TiO2粉末(60mg)、[(CN)(H2O)Cob(III)7COOH]Cl(6mg，0.005mmol)和RhB(2mg，0.005mmol)，超声分散于4mL无水甲醇中，室温下搅拌4h，离心，并用甲醇洗至上清液为无色，真空干燥，得淡粉色复合光催化剂B12-TiO2-RhB粉末57mg。
(二)检测结果
图4是P25型TiO2和B12-TiO2-RhB的X-射线粉末衍射图。通过对比可以确定，经维生素B12衍生物和RhB修饰后得到的B12-TiO2-RhB复合物在相应的位置也出现尖锐的特征吸收峰，证明了两种功能分子对二氧化钛的修饰没有改变二氧化钛的晶型结构。
图5是P25型TiO2(a)和B12-TiO2-RhB(b)的甲醇分散液在室温下静置1h的照片。通过对比可以确定，复合催化剂B12-TiO2-RhB在甲醇中有良好的分散性能，能够形成稳定的分散液。这种良好的分散性能将有利于催化剂催化效率的提高。
实施例2在可见光驱动下具有催化活性的复合光催化剂B12-TiO2-RhB的应用
将B12-TiO2-RhB(3mg)、DDT(2.4×10-3M)和三乙醇胺(0.2M)分散于5mL的无水甲醇中，通入氮气除氧后，在氮气保护下，可见光照射下反应1h。反应结束后离心除去催化剂B12-TiO2-RhB，上清液减压下旋除溶剂甲醇，得催化粗产物。
催化粗产物溶于10ml二氯甲烷，用去离子水(10ml)萃取三次，最后二氯甲烷层减压下旋除溶剂二氯甲烷，得到催化产物，干燥，产物中加入一定量1,4-二氧六环作为内标物，利用核磁氢谱对反应物转化率及产物产率进行分析，确定DDT转化率为100％，产物为DDD，产率为93％。图6是可见光驱动下催化降解DDT的反应式。
Claims (8)
1.一种在可见光驱动下具有催化活性的复合光催化剂，其特征在于：所述的复合光催化剂是B12-TiO2-RhB。
2.权利要求1所述的一种在可见光驱动下具有催化活性的复合光催化剂的制备方法，其特征在于，包括如下步骤：将适量的含有羧基的维生素B12衍生物和光敏剂RhB溶于甲醇溶液中，加入适量的TiO2纳米球，超声分散，常温搅拌，离心，产物用甲醇洗涤至无色，真空干燥，得目标产物。
3.根据权利要求2所述的制备方法，其特征在于：按质量比，含有羧基的维生素B12衍生物:光敏剂RhB:TiO2＝3:1:30。
4.根据权利要求2所述的制备方法，其特征在于：所述的含有羧基的维生素B12衍生物为[(CN)(H2O)Cob(III)7COOH]Cl。
5.根据权利要求2所述的制备方法，其特征在于：所述的TiO2纳米球为P25型的TiO2。
6.权利要求1所述的一种在可见光驱动下具有催化活性的复合光催化剂在可见光驱动下降解有机卤代物中的应用。
7.根据权利要求6所述的应用，其特征在于，方法如下：常温下，将权利要求1所述的复合光催化剂B12-TiO2-RhB，超声分散于含有有机卤代物的甲醇溶液中，再加三乙醇胺，超声分散，反应液通入氮气除氧，并在氮气保护下可见光照射反应。
8.根据权利要求6或7所述的应用，其特征在于，所述的有机卤代物是2,2-双(4-氯苯基)-1,1,1-三氯乙烷。
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Cited By (4)
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| CN109622040A (zh) * | 2019-01-23 | 2019-04-16 | 辽宁大学 | 一种催化三氯甲苯转化成酯的可见光催化剂及其制备方法和应用 |
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| CN110172034B (zh) * | 2019-05-31 | 2021-04-02 | 江苏强盛功能化学股份有限公司 | 一种芳乙基过氧化氢的制备方法 |
| CN111229326A (zh) * | 2020-03-09 | 2020-06-05 | 辽宁大学 | 一种新型催化水光解制氢复合光催化剂的制备方法及其应用 |
| CN111229326B (zh) * | 2020-03-09 | 2022-07-19 | 辽宁大学 | 一种催化水光解制氢复合光催化剂的制备方法及其应用 |
| CN111229328A (zh) * | 2020-03-25 | 2020-06-05 | 辽宁大学 | 一种辅酶B12修饰Ti3C2(OH)X纳米片复合光催化剂及其制备方法和应用 |
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