CN114210355A - 一种富缺陷三维多孔原位碳掺杂g-C3N4催化剂的制备方法 - Google Patents
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Abstract
本发明公开了一种富缺陷三维多孔原位碳掺杂g‑C3N4催化剂的制备方法，该方法以三维网络三聚氰胺‑三聚氰酸超分子为前驱体以获得三维多孔结构g‑C3N4样品，并在合成过程中加入三氨基嘧啶，采用一步煅烧法制备具有三维多孔结构的原位碳掺杂g‑C3N4样品；再将原位碳掺杂g‑C3N4样品与硼氢化钠混合均匀，经退火处理得到富缺陷三维多孔原位碳掺杂g‑C3N4催化剂。在可见光照射下，该催化剂表现出了优异且稳定的光催化降解有机污染物和产氢活性。该制备方法工艺简单、原料成本低、易于大规模生产，在环境领域具有良好的应用前景。
Description
技术领域
本发明属于可见光催化材料的制备技术领域，具体涉及一种富缺陷三维多孔原位碳掺杂g-C3N4催化剂的制备方法。
背景技术
在众多催化剂中，石墨相氮化碳（g-C3N4）是一种二维层状非金属光催化材料，能够吸收可见光，热稳定性及化学稳定性良好，并且无毒、来源丰富、制备工艺较为简单。在光催化产氢、水氧化、有机物降解、光合成以及二氧化碳还原等领域具有重要研究价值。然而目前文献报道的g-C3N4在光催化反应中仍然面临比表面积小、禁带宽度较宽、光生载流子难以有效分离等问题。对其g-C3N4进行形貌调控、掺杂以及在其框架中引入氮缺陷则能够有效解决上述问题，因而受到研究人员广泛关注。
目前，文献已报道的碳掺杂大多是采用碳桥联的方式来提升g-C3N4的催化性能。而引入氮缺陷的方法通常涉及多步操作过程，并且需要借助苛刻的反应条件（如还原气氛高温处理等）。不仅实验过程危险难以实际应用，其产生缺陷多为不均匀的表面缺陷，而且缺陷程度难以调控。此外，大多形貌调控方式也是操作复杂，不易大规模生产。因此，如何通过简便的合成方法制备氮缺陷程度可控的三维多孔富缺陷碳掺杂g-C3N4催化剂，从而进一步提高材料的光催化活性具有重大研究意义。
发明内容
本发明解决的技术问题是提供了一种简便、易大规模生产的具有优异且稳定的可见光催化活性的富缺陷三维（3D）多孔原位碳掺杂g-C3N4催化剂的制备方法，该方法以三聚氰胺和三聚氰酸为前驱体以获得三维多孔结构催化剂，并在合成过程中加入三氨基嘧啶，采用一步煅烧法制备具有三维多孔结构的原位碳掺杂g-C3N4；然后将原位碳掺杂g-C3N4与硼氢化钠混合均匀，经干燥退火处理，即制得缺陷可控的氮缺陷三维多孔结构的原位碳掺杂g-C3N4催化剂；在可见光下，该g-C3N4催化剂表现出了优异且稳定的光催化降解有机污染物和产氢性能。
本发明为解决上述技术问题采用如下技术方案，一种富缺陷三维多孔原位碳掺杂g-C3N4催化剂的制备方法，其特征在于具体步骤为：
步骤S1：将三聚氰胺和三聚氰酸加入到去离子水中配制三聚氰胺-三聚氰酸超分子前体溶液，搅拌使其分散均匀；
步骤S2：向步骤S1得到的三聚氰胺-三聚氰酸超分子前体溶液中添加三氨基嘧啶，继续搅拌过夜，再转移至培养皿中于60℃进行干燥得到前体物；
步骤S3：将步骤S2干燥后的前驱物研磨，在空气条件下于520-600℃退火处理2-4h得到棕黄色的三维多孔原位碳掺杂g-C3N4；
步骤S4：将步骤S3得到的三维多孔原位碳掺杂g-C3N4与硼氢化钠混合均匀，在空气条件下于300-400℃退火处理1-2h得到目标产物黄色的富缺陷三维多孔原位碳掺杂g-C3N4催化剂。
进一步限定，步骤S1中所述三聚氰胺与三聚氰酸的投料摩尔比为1:1，步骤S2中所述三氨基嘧啶的投料量为三聚氰胺与三聚氰酸总质量的1-20倍。
进一步限定，步骤S4中所述三维多孔原位碳掺杂g-C3N4与硼氢化钠的质量比为10:1。
本发明与现有技术相比具有以下有益效果：
1、本发明制得的富缺陷三维多孔原位碳掺杂g-C3N4催化剂缺陷可控，具有良好的可见光相应和较大的比表面积，为光催化反应提供更多的反应活性位点，表现出优异且稳定的的可见光催化性能，可广泛应用于可见光催化产氢和持久性有机污染物的降解；
2、本发明制备的富缺陷三维多孔原位碳掺杂g-C3N4催化剂的方法原料成本低廉、制备工艺简单且易于大规模生产。
附图说明
图1是本发明的制备工艺流程图；
图2是本发明实施例1制备的富缺陷3D多孔原位碳掺杂g-C3N4催化剂的场发射电子扫描显微镜图；
图3是本发明实施例1制备的富缺陷3D多孔原位碳掺杂g-C3N4催化剂的有机污染物双氯酚酸的去除效果图；
图4是本发明实施例2制备的富缺陷3D多孔原位碳掺杂g-C3N4催化剂的可见光催化产氢效果图。
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
首先，取2.52g三聚氰胺和2.58g三聚氰酸溶于100mL去离子水中，搅拌至均匀；然后向上述溶液中加入30mg三氨基嘧啶，继续搅拌过夜；随后将搅拌均匀的溶液转移至玻璃皿中，于60℃干燥12h；将所得前体物研磨，于550℃退火处理4h，即得到棕黄色的3D多孔原位碳掺杂g-C3N4样品；将0.5g原位碳掺杂g-C3N4样品与0.05g硼氢化钠混合均匀，于300℃退火处理1h即得到黄色的富缺陷3D多孔原位碳掺杂g-C3N4催化剂。
实施例2
首先，取2.52g三聚氰胺和2.58g三聚氰酸溶于80mL去离子水中，搅拌至均匀；然后向上述溶液中加入80mg三氨基嘧啶，继续搅拌过夜；随后将搅拌均匀溶液转移至玻璃皿中，于60℃干燥12h；将所得前体物研磨，于600℃退火处理4h，即得到棕黄色的3D多孔原位碳掺杂g-C3N4样品；将0.5g原位碳掺杂g-C3N4样品与0.1g硼氢化钠混合均匀，于350℃退火处理2h即得到黄色的富缺陷3D多孔原位碳掺杂g-C3N4催化剂。
实施例3
取20mg实施例1中制备的富缺陷3D多孔原位碳掺杂g-C3N4催化剂分散与60mL浓度为10mg/L的四环素溶液，经暗光搅拌30min，开启光源、计时，分别在特定时间点取样过滤分析，在可见光下反应90min后，溶液中四环素的降解率为100%，效果详见图3。
实施例4
取50mg实施例2中制备的富缺陷3D多孔原位碳掺杂g-C3N4催化剂分散到100mL三乙醇胺的水溶液（10wt%）中，加入0.2mL 5mmol/L的氯铂酸溶液，黑暗条件下超声30min，再加入到反应器中，然后将反应器与气路循环系统连接，使用真空泵对反应系统抽真空处理1h排除系统内的空气，然后开启光源，产生的气体使用气相色谱仪在线监测，采样间隔30min，3h的光催化产氢效果详见图4。
以上显示和描述了本发明的基本原理，主要特征和优点，在不脱离本发明精神和范围的前提下，本发明还有各种变化和改进，这些变化和改进都落入要求保护的本发明的范围。
Claims (3)
1.一种富缺陷三维多孔原位碳掺杂g-C3N4催化剂的制备方法，其特征在于具体步骤为：
步骤S1：将三聚氰胺和三聚氰酸加入到去离子水中配制三聚氰胺-三聚氰酸超分子前体溶液，搅拌使其分散均匀；
步骤S2：向步骤S1得到的三聚氰胺-三聚氰酸超分子前体溶液中添加三氨基嘧啶，继续搅拌过夜，再转移至培养皿中于60℃进行干燥得到前体物；
步骤S3：将步骤S2干燥后的前驱物研磨，在空气条件下于520-600℃退火处理2-4h得到棕黄色的三维多孔原位碳掺杂g-C3N4；
步骤S4：将步骤S3得到的三维多孔原位碳掺杂g-C3N4与硼氢化钠混合均匀，在空气条件下于300-400℃退火处理1-2h得到目标产物黄色的富缺陷三维多孔原位碳掺杂g-C3N4催化剂。
2.根据权利要求1所述的富缺陷三维多孔原位碳掺杂g-C3N4催化剂的制备方法，其特征在于：步骤S1中所述三聚氰胺与三聚氰酸的投料摩尔比为1:1，步骤S2中所述三氨基嘧啶的投料量为三聚氰胺与三聚氰酸总质量的1-20倍。
3.根据权利要求1所述的富缺陷三维多孔原位碳掺杂g-C3N4催化剂的制备方法，其特征在于：步骤S4中所述三维多孔原位碳掺杂g-C3N4与硼氢化钠的质量比为10:1。
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| CN115282996A (zh) * | 2022-07-11 | 2022-11-04 | 华东理工大学 | 一种高效光解水产氢的p,s,b回填氮空位氮化碳材料的制备方法及应用 |
| CN116212916A (zh) * | 2022-12-07 | 2023-06-06 | 新乡医学院 | 一种钴锰基复合催化剂及其制备方法和在活化过氧单硫酸盐降解抗生素中的应用 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115282996A (zh) * | 2022-07-11 | 2022-11-04 | 华东理工大学 | 一种高效光解水产氢的p,s,b回填氮空位氮化碳材料的制备方法及应用 |
| CN116212916A (zh) * | 2022-12-07 | 2023-06-06 | 新乡医学院 | 一种钴锰基复合催化剂及其制备方法和在活化过氧单硫酸盐降解抗生素中的应用 |
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