CN110270365A - 一种氮化碳/氯氧化镧复合材料的制备与应用 - Google Patents
一种氮化碳/氯氧化镧复合材料的制备与应用 Download PDFInfo
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Abstract
本发明具体涉及一种C3N4/LaOCl复合材料的制备方法和应用，其属于光催化领域。本发明将低熔点的水溶性氯化物熔盐和适量三聚氰胺及氧化镧充分混合，在熔盐熔融温度下一步煅烧合成所述C3N4/LaOCl复合材料。本发明采用一步熔盐法制备C3N4/LaOCl复合材料，无需引入模板，简单易行，熔盐可水洗回收，成本经济，环境友好，易于大规模工业化生产。所得C3N4/LaOCl复合材料呈淡黄色、二维片状形貌，能够在可见光照下光催化水全分解生成H2和O2，生成的氢气和氧气物质的量之比接近于水全分解的化学计量比2:1，具有良好应用前景。
Description
技术领域
本发明涉及一种可见光响应的高效稳定、低成本光催化材料及其制备方法和应用，具体涉及一种C3N4/LaOCl复合材料及其制备方法和应用。
背景技术
近年来，氮化碳（C3N4）作为新兴的共轭聚合物光催化材料备受关注，在水分解、光催化CO2还原、光催化有机选择性合成和有机污染物降解等方面有大量研究报道，但C3N4光生电子空穴易复合，光催化效率低，光催化分解水制氢的研究多是在三乙醇胺等电子授体存在下的产氢半反应，不能实现水的完全分解，影响了其实际应用。研究表明，通过异质结将两种能带位置匹配的催化材料结合起来构筑的复合材料，通过结间的电荷传递，可加速光生载流子分离与迁移，提高光量子效率，进而实现较高效率的光催化水全分解，提高光催化效率。氯氧化镧（LaOCl）是一种重要的发光基质，具有较高的光吸收和传能效率，在彩色显示、催化、光电转换、气敏等领域均有广泛的应用，作为光催化材料，较宽的带隙影响了其可能的实际应用。将能带位置匹配的C3N4和LaOCl进行复合构建复合光催化剂，利用异质结间的电子空穴传递，实现光生载流子的有效分离，将有望得到一种新型高效的全解水光催化剂。因此，开发简单易行，成本经济，环境友好的C3N4/LaOCl复合光催化材料的制备方法将具有重要意义。
发明内容
本发明的目的在于提供一种C3N4/LaOCl复合材料的制备方法及其应用，该制备方法简单易行，成本经济，环境友好，易于大规模推广。本发明所制备的C3N4/LaOCl复合材料具有催化活性高和稳定性好的优点，可应用于光催化水全分解制氢。
为实现上述目的，本发明采用如下技术方案：
一种C3N4/LaOCl复合材料的制备方法，其是以低熔点水溶性氯化物熔盐、三聚氰胺和氧化镧为原料，经熔盐法一步合成。其具体是将低熔点水溶性氯化物熔盐、三聚氰胺和氧化镧置于研钵内充分混合并研磨均匀后，放入带盖的刚玉坩埚中，将坩埚置于马弗炉内，经400~600 ℃处理1~5 h后，自然降温至室温，将所得混合物经去离子水洗涤至离子浓度<10ppm，再于40~120 ℃干燥3~12 h，得到淡黄色复合材料C3N4/LaOCl粉末。
其中，所用低熔点水溶性氯化物熔盐、三聚氰胺（C3N6H6）和氧化镧（La2O3）的质量比为(0.1~10):(0.1~10):(0.1~10)。
所述低熔点水溶性氯化物熔盐为氯化锂和氯化钾的混合物，两者的质量比为KCl:LiCl=(0.1~10):1，其熔点范围为353~771℃。
所制得的C3N4/LaOCl复合材料可应用于光催化，尤其是光催化水全分解制氢中。
本发明的显著优点在于：
（1）本发明首次制备了复合材料C3N4/LaOCl。
（2）本发明采用一步熔盐法，所制备的复合物中两组分之间具有密切的接触，有利于光生电子和空穴的传输与分离，且制备工艺简单，成本低。
（3）本发明产物为水全分解光催化剂，其在可见光照射下在纯水中（无任何牺牲试剂）能够分解水产生氢气和氧气，且所生成的氢气和氧气的物质的量之比接近水全分解的化学计量比2:1。
附图说明
图1为实施例1所制备C3N4/LaOCl复合材料的X射线粉末衍射图；
图2为实施例1所制备C3N4/LaOCl复合材料的扫描电镜图；
图3为实施例1所制备C3N4/LaOCl复合材料的紫外-可见漫反射光谱图；
图4为实施例1所制备C3N4/LaOCl作为催化剂可见光催化水全分解制氢的活性图；
图5为实施例1所制备C3N4/LaOCl作为催化剂可见光催化水全分解制氢的活性稳定性图。
具体实施方式
为了使本发明所述的内容更加便于理解，下面结合具体实施方式对本发明所述的技术方案做进一步的说明，但是本发明不仅限于此。
实施例1 复合材料C3N4/LaOCl的制备
称取1.5 g氯化锂、1.5 g氯化钾、1.0 g三聚氰胺和0.5 g氧化镧置于研钵中充分研磨混合均匀后，放入带盖子的刚玉坩埚中，置于马弗炉内经550 ℃恒温处理3 h，自然降温至室温后，所得混合物经去离子水洗涤至离子浓度<10 ppm，60 ℃干燥6 h，得到复合材料C3N4/LaOCl。
图1为本实施例所制备的C3N4/LaOCl样品的X射线粉末衍射图。从图中可以发现样品呈现四方LaOCl（JCPDS:08~0477）的特征衍射峰，没有发现C3N4的特征衍射峰。
图2为本实施例所制备的C3N4/LaOCl样品的扫描电镜图。由图可见，C3N4/LaOCl样品呈长约5~20 μm，宽约1~10 μm的二维片状形貌。
图3为本实施例所制备的C3N4/LaOCl样品的紫外-可见吸收光谱图。由图可以发现，复合材料C3N4/LaOCl相较于单一的LaOCl具有明显增强的光吸收，其吸收带边在435 nm左右。
实施例2 复合材料C3N4/LaOCl的制备
称取1.0 g氯化锂、1.0 g氯化钾、1.0 g三聚氰胺和1.0 g氧化镧置于研钵中充分研磨混合均匀后，放入带盖的刚玉坩埚中，置于马弗炉内经500 ℃恒温处理2 h，自然降温至室温后，用去离子水洗涤至离子浓度<10 ppm，于60 ℃干燥6 h，得到复合材料C3N4/LaOCl。
实施例3 样品C3N4的制备
称取1.5 g氯化锂、1.5 g氯化钾和1.0 g三聚氰胺置于研钵中充分研磨混合均匀后，放入带盖的刚玉坩埚中，置于马弗炉内经500 ℃恒温处理2 h，自然降温至室温后，用去离子水洗涤至离子浓度<10 ppm，于60 ℃干燥6 h，得到C3N4。
实施例4 样品LaOCl的制备
称取1.5 g氯化锂、1.5 g氯化钾和0.5 g氧化镧置于研钵中充分研磨混合均匀后，放入带盖子的刚玉坩埚中，置于马弗炉内经550 ℃恒温处理3 h，自然降温至室温后，所得混合物经去离子水洗涤至离子浓度<10 ppm，60 ℃干燥6 h，得到LaOCl。
实施例5
称取1.5 g氯化锂（或氯化钾）、1.0 g三聚氰胺和0.5 g氧化镧置于研钵中充分研磨混合均匀后，放入带盖子的刚玉坩埚中，置于马弗炉内经550 ℃恒温处理3 h，自然降温至室温后，发现无法得到复合材料C3N4/LaOCl。
实施例6
称取1.5 g氯化锂、1.5 g氯化钾、1.0 g三聚氰胺和0.5 g氧化镧置于研钵中充分研磨混合均匀后，放入带盖子的刚玉坩埚中，置于马弗炉内经620~750 ℃恒温处理3 h，自然降温至室温后，发现无法得到复合材料C3N4/LaOCl。
实施例7 复合材料C3N4/LaOCl光催化水全分解制氢性能
将实施例1制得的C3N4/LaOCl样品用于光催化水全分解制氢，同时以实施例3制得的C3N4和实施例4制得的LaOCl作为对照样。在光催化全分解水制氢反应之前，采用光沉积法在样品表面沉积其重量0.5 wt.% Pt和0.1 wt.% Co作为助催化剂，具体步骤为：取100 mg样品分散于100 ml去离子水中，滴加1 mL甲醇、一定量的H2PtCl6（基于Pt的含量）和CoCl2（基于Co的含量），抽真空后光照1 h，经去离子水洗涤，干燥后得到Pt和Co修饰的样品。光催化水全分解的反应是在密封的循环体系中进行，反应器体积约为250 mL，以装配400 nm滤光片的300 W氙灯作为光源。称取50 mg Pt和Co修饰的样品置于反应器中，然后加入100 mL超纯水，磁力搅拌均匀，打开机械泵将反应体系抽至0.1MPa真空，打开光源和气体循环泵。每隔一段时间通过四通阀将气相产物导入色谱在线检测分析，结果如图4。由图中可见，C3N4/LaOCl样品光照4 h产生32.1 μmol H2与15.2 μmol O2，接近水全分解的化学计量比2：1。相同条件下LaOCl则未检测到水分解产物，C3N4只检测到产生少量H2。
实施例8 复合材料C3N4/LaOCl光催化水全分解制氢活性稳定性
为了考察复合材料C3N4/LaOCl光催化分解水产氢的活性稳定性，按实施例7的光催化产氢活性实验进行循环测试，每个循环测试周期为4 h，即光催化产氢反应4 h后关灯、关气体循环泵，打开机械泵将密闭反应体系抽真空30 min，再打开光源和气体循环泵开始下个活性测试周期，如此反复循环5次，结果如图5。由图中可见，每个活性测试周期随着光照时间的延长，检测到的氢气和氧气的产量稳定增加，不同测试周期间样品的产氢活性没有明显变化，表明C3N4/LaOCl样品具备良好的活性稳定性。
以上所述仅为本发明的较佳实施例，凡依本发明申请专利范围所做的均等变化与修饰，皆应属本发明的涵盖范围。
Claims (5)
1.一种C3N4/LaOCl复合材料的制备方法，其特征在于：以低熔点水溶性氯化物熔盐、三聚氰胺和氧化镧为原料，在熔盐熔融温度下一步煅烧合成复合材料C3N4/LaOCl。
2.根据权利要求1所述的C3N4/LaOCl复合材料的制备方法，其特征在于：所用低熔点水溶性氯化物熔盐、三聚氰胺和氧化镧的质量比为(0.1~10):(0.1~10):(0.1~10)。
3.根据权利要求1或2所述的C3N4/LaOCl复合材料的制备方法，其特征在于：所述低熔点水溶性氯化物熔盐为氯化锂和氯化钾的混合物，两者的质量比为KCl:LiCl=(0.1~10):1，其熔点范围为353~771℃。
4.根据权利要求1所述的C3N4/LaOCl复合材料的制备方法，其特征在于：所述煅烧的温度为400~600 ℃，处理时间为1~5 h。
5.一种如权利要求1~4所述方法制得的C3N4/LaOCl复合材料在光催化中的应用，其特征在于：用于光催化水全分解制氢。
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