CN107159184B - 水热辅助制备介孔结构LiNb3O8光催化剂的方法 - Google Patents
水热辅助制备介孔结构LiNb3O8光催化剂的方法 Download PDFInfo
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Abstract
本发明公开了一种水热辅助制备介孔结构LiNb3O8光催化剂的方法，属于三铌酸锂光催化剂的合成技术领域。本发明的技术方案要点为：将五氧化二铌分散于水溶液中，再将一水合氢氧化锂加入到上述溶液中搅拌混合均匀得到白色悬浊液；将得到的白色悬浊液转移至聚四氟乙烯内衬的反应釜中，再将反应釜密封后置于干燥箱中于260℃水热反应24h；将水热反应产物取出后通过去离子水和无水乙醇清洗至中性，然后于60‑250℃干燥10‑48h得到白色粉体；将得到的白色粉体于700‑900℃退火2‑12h得到介孔结构LiNb3O8光催化剂。本发明首次合成了介孔结构的LiNb3O8粉体，该粉体在紫外光源下可有效催化降解有机污染物，并且本发明合成工艺简单，制得的粉体具有优异的催化活性。
Description
技术领域
本发明属于三铌酸锂光催化剂的合成技术领域，具体涉及一种水热辅助制备介孔结构LiNb3O8光催化剂的方法。
背景技术
染料废水是日常污染严重的工业废水之一，具有种类繁杂、颜色深和难生物降解等特点，严重污染水质环境，进而威胁到大自然生态系统和人们的身体健康。常规的污染处理方法效果不理想，自发现TiO2具有良好的光降解有机物性能以来，半导体材料光催化降解技术日趋受到关注，寻找高效的光催化材料一直是科学家和各国政府的工作重点。其中铌酸盐，作为一种环境治理和新能源材料得到了广泛的研究，主要包括：(Na, K)NbO3,BiNbO4, LiNbO3和LiNb3O8。在这些材料当中，LiNb3O8作为一种新型的氧化物材料，在锂电池、超级电容器和光解水制氢方面有着很好的应用前景。但是传统的固相法制备工艺不利于纯相的获得，同时获得材料颗粒尺寸大，活性位少不利于光催化应用。研究表明，介孔结构光催化材料可以提供更大的比表面积、更多的活性位，相对于传统结构表现出更加优异的光催化性能。水热法是一个常见的纳米材料制备工艺，有制备温度低，环境友好和颗粒尺寸分布均匀等优点。然而，目前尚没有关于水热辅助制备介孔结构LiNb3O8光催化剂的相关报道。
发明内容
本发明解决的技术问题是提供了一种制备工艺简单、产品性能优良且成本相对低廉的水热辅助制备介孔结构LiNb3O8光催化剂的方法。
本发明为解决上述技术问题采用如下技术方案，水热辅助制备介孔结构LiNb3O8光催化剂的方法，其特征在于具体步骤为：
（1）将0.4666g五氧化二铌分散于35mL水溶液中，再将1.175g一水合氢氧化锂加入到上述溶液中搅拌混合均匀得到白色悬浊液；
（2）将得到的白色悬浊液转移至聚四氟乙烯内衬的反应釜中，再将反应釜密封后置于干燥箱中于260℃水热反应24h；
（3）将水热反应产物取出后通过去离子水和无水乙醇清洗至中性，然后于60-250℃干燥10-48h得到白色粉体；
（4）将得到的白色粉体于700-900℃退火2-12h得到介孔结构LiNb3O8光催化剂。
本发明首次合成了介孔结构的LiNb3O8粉体，该粉体在紫外光源下可有效催化降解有机污染物，并且本发明合成工艺简单，制得的粉体具有优异的催化活性，800℃煅烧获得的介孔结构LiNb3O8在500W紫外光下30min对亚甲基蓝的降解率为90%，其可用于工业污水的治理和染料废水的降解等，应用范围较广。
附图说明
图1是本发明实施例1-4制得的介孔结构LiNb3O8粉末的X射线衍射图；
图2是本发明实施例1-4制得的介孔结构LiNb3O8粉末的SEM图，其中（a）700℃退火2h，（b）800℃退火2h；（c）850℃退火2h；（d）900℃退火2h；
图3是本发明实施例1-4制得的介孔结构LiNb3O8粉末对亚甲基蓝的光催化降解曲线，其中光催化剂量为1g/L，取样间隔为30min。
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
将0.4666g五氧化二铌（Nb2O5）分散于35mL去离子水中，再将1.175g一水合氢氧化锂（LiOH·H2O）溶于上述溶液中，搅拌30min后得到白色悬浊液，将得到的白色悬浊液转移到聚四氟乙烯内衬的反应釜中，密封后置于干燥箱中于260℃水热反应24h，反应完成后自然冷却至室温，将产物取出后通过去离子水和无水乙醇洗至中性，然后于60℃干燥12h得到白色粉体，将得到的白色粉体置于马弗炉中于700℃煅烧2h得到白色介孔结构LiNb3O8粉末。用该粉末（1g/L）降解5mg/L的亚甲基蓝溶液，室温下超声分散10min后，紫外光下反应60min，降解率达到了92%。
实施例2
其他条件同实施例1，将得到的白色粉体置于马弗炉中于800℃退火2h得到白色介孔结构LiNb3O8粉末。用该粉末（1g/L）降解5mg/L的亚甲基蓝溶液，室温下超声分散10min后，紫外光下反应30min，降解率达到了90%。
实施例3
其他条件同实施例1，将得到的白色粉体置于马弗炉中于850℃退火2h得到白色介孔结构LiNb3O8粉末。用该粉末（1g/L）降解5mg/L的亚甲基蓝溶液，室温下超声分散10min后，紫外光下反应90min，降解率达到了88%。
实施例4
其他条件同实施例1，将得到的白色粉体置于马弗炉中于900℃退火2h得到白色介孔结构的LiNb3O8粉末。用该粉末（1g/L）降解5mg/L的亚甲基蓝溶液，室温下超声分散10min后，紫外光下反应90min，降解率达到了93%。
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 (1)
1.水热辅助制备介孔结构LiNb3O8光催化剂的方法，其特征在于具体步骤为：
（1）将0.4666g五氧化二铌分散于35mL水溶液中，再将1.175g一水合氢氧化锂加入到上述溶液中搅拌混合均匀得到白色悬浊液；
（2）将得到的白色悬浊液转移至聚四氟乙烯内衬的反应釜中，再将反应釜密封后置于干燥箱中于260℃水热反应24h；
（3）将水热反应产物取出后通过去离子水和无水乙醇清洗至中性，然后于60-250℃干燥10-48h得到白色粉体；
（4）将得到的白色粉体于700-900℃退火2-12h得到介孔结构LiNb3O8光催化剂。
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| CN108283941B (zh) * | 2017-09-26 | 2020-06-12 | 河海大学 | 用于污水处理厂尾水中总氮处理的非线性光催化膜及其应用 |
| CN110092414B (zh) * | 2018-01-30 | 2021-01-26 | 北京大学 | 一类具有特殊微观结构的金属氧化物材料及其制备方法 |
| CN108865108B (zh) * | 2018-08-03 | 2021-04-16 | 广东工业大学 | 一种铌酸盐变色材料及其制备方法 |
| CN109589963B (zh) * | 2018-12-12 | 2020-05-26 | 常州大学 | 一种铌酸锂型氧化物/凹凸棒石非线性光学复合光催化材料及其制备方法与应用 |
| CN109718756B (zh) * | 2019-03-07 | 2021-11-05 | 河南师范大学 | 一种正交相五氧化二铌光催化材料的制备方法 |
| CN113750985B (zh) * | 2021-09-23 | 2024-03-15 | 上海科技大学 | 一种用于降解亚甲基蓝的催化剂及其制备方法和应用 |
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