CN113976157A - 一种三维多孔原位碳掺杂g-C3N4催化剂的制备方法 - Google Patents
一种三维多孔原位碳掺杂g-C3N4催化剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种三维多孔原位碳掺杂g‑C3N4催化剂的制备方法，属于光催化产氢和降解环境污染物催化剂的制备技术领域，本发明的制备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。在可见光照射下，该催化剂具有优异且稳定的光催化产氢和有机污染物降解性能。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
本发明属于光催化产氢和降解环境污染物催化剂的制备技术领域，具体涉及一种三维多孔原位碳掺杂g-C3N4催化剂的制备方法。
背景技术
近年来，能源匮乏和环境污染是影响人类社会发展的重大问题。利用光催化剂将取之不尽的太阳能转化为人类可直接利用的能量，将各种有机和无机的污染物完全矿化和降解，是目前可再生清洁能源研究的一个方向。
在众多光催化剂中，具有独特结构的石墨相氮化碳g-C3N4由于其具有良好的光催化性能，成为了目前研究的热点。相比于其它的光催化剂，它的优点十分突出：能够吸收可见光、热稳定性和化学稳定性良好，并且无毒、来源丰富、制备成型工艺也较为简单。然而，传统的体相g-C3N4存在光生载流子复合率高，光吸收范围有限、比表面积低等问题，导致其光催化效果不够理想，这在很大程度上限制了它的实际应用。因此，开发具有高效光催化活性的g-C3N4催化剂具有重要意义。
目前，国内外的科研人员做了大量改性工作来提升g-C3N4的光催化性能。其中，将二维（2D）g-C3N4组装成三维（3D）多孔网状聚集体，不仅能够有效阻止g-C3N4结构层的堆积，促进污染物的扩散吸附，还有利于吸附污染物后的固液分离。因此，3D多孔结构g-C3N4材料在光催化领域具有广泛的应用前景。目前，针对3D多孔结构g-C3N4催化剂的研究尚处于起步阶段，催化剂自身依然存在光生电荷复合率高、光吸收范围有限等缺点，迫切需要对其进行改性处理以进一步提升其光催化性能，而对3D多孔结构g-C3N4进行掺杂改性，将能够有效解决以上技术问题。
发明内容
本发明解决的技术问题是提供了一种具有优异可见光催化产氢和降解有机污染物的三维多孔原位碳掺杂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催化剂；在可见光下，该催化剂具有优异且稳定的光催化产氢和有机污染物降解性能，较传统g-C3N4具有更宽的光谱工作范围。
本发明为解决上述技术问题采用如下技术方案，一种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：配制三聚氰胺和三聚氰酸超分子前体溶液
分别将三聚氰胺和三聚氰酸加入去离子水中，搅拌使其分散均匀得到三聚氰胺和三聚氰酸超分子前体溶液；
步骤S2：三维多孔原位碳掺杂g-C3N4催化剂的制备
向步骤S1得到的三聚氰胺和三聚氰酸超分子前体溶液中加入三氨基嘧啶，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，然后将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，所述三聚氰胺与去离子的投料配比为2.52g:50-100mL。
进一步限定，步骤S2中所述三氨基嘧啶与三聚氰胺的投料配比为10-100mg:2.52g。
本发明与现有技术相比具有以下优点和有益效果：
1、本发明制得的三维多孔原位碳掺杂g-C3N4催化剂具有优异且稳定的的可见光催化性能，较传统g-C3N4催化剂具有更宽的光谱工作范围，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；
3、本发明制备的三维多孔原位碳掺杂g-C3N4催化剂具有较大的比表面积，为光催化反应提供更多的反应活性位点，进而具有优异的光催化活性。
附图说明
图1是本发明的制备工艺流程图；
图2是本发明制备的三维多孔原位碳掺杂g-C3N4催化剂的场发射电子扫描显微镜图；
图3是本发明制备的三维多孔原位碳掺杂g-C3N4催化剂的可见光催化产氢效果图；
图4是本发明制备的三维多孔原位碳掺杂g-C3N4催化剂的有机污染物双氯酚酸的去除效果图。
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，搅拌至混合均匀得到三聚氰胺和三聚氰酸超分子前体溶液；然后向上述三聚氰胺和三聚氰酸超分子前体溶液中加入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；将干燥后的前体物研磨，于550℃退火处理4h，即得到棕黄色的三维多孔原位碳掺杂g-C3N4样品。
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，搅拌至混合均匀得到三聚氰胺和三聚氰酸超分子前体溶液；然后向上述三聚氰胺和三聚氰酸超分子前体溶液中加入60mg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；将干燥后的前体物研磨，于600℃退火处理4h，即得到棕黄色的三维多孔原位碳掺杂g-C3N4样品。。
实施例3
将50mg实施例1中制备的三维多孔原位碳掺杂g-C3N4样品加入到100mL三乙醇胺的水溶液（10wt%）中，再加入0.2mL 5mmol的氯铂酸，黑暗条件下超声30min，然后加入到反应器中，再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，然后开启氙灯，产生的气体使用气相色谱仪在线监测，采样间隔30min，检测器为TCD热导检测器，载气使用高纯氮气，产氢效果详见图3。
实施例4
取80mL质量浓度为10mg/L的双氯酚酸溶液，再加入实施例2中制备的三维多孔原位碳掺杂g-C3N4样品，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120min后，溶液中双氯酚酸的去除率为100%，降解效果详见图4。
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 (3)
1.一种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：配制三聚氰胺和三聚氰酸超分子前体溶液
分别将三聚氰胺和三聚氰酸加入去离子水中，搅拌使其分散均匀得到三聚氰胺和三聚氰酸超分子前体溶液；
步骤S2：三维多孔原位碳掺杂g-C3N4催化剂的制备
向步骤S1得到的三聚氰胺和三聚氰酸超分子前体溶液中加入三氨基嘧啶，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，然后将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催化剂。
2.根据权利要求1所述的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，所述三聚氰胺与去离子水的投料配比为2.52g:50-100mL。
3.根据权利要求1所述的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S2中所述三氨基嘧啶与三聚氰胺的投料配比为10-100mg:2.52g，制得的三维多孔原位碳掺杂g-C3N4催化剂具有优异且稳定的的可见光催化性能以及更宽的光谱工作范围，能够应用于可见光催化产氢和持久性有机污染物的降解。
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