CN114405550A - 一种NH2-UiO-66/CdIn2S4光催化剂及其制备方法和应用 - Google Patents
一种NH2-UiO-66/CdIn2S4光催化剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明属于催化制氢技术领域，尤其涉及一种NH2‑UiO‑66/CdIn2S4光催化剂及其制备方法和应用。制备方法包括如下步骤：将NH2‑UiO‑66晶体溶于去离子水中，然后分别加入2.5水合氯化镉，四水合氯化铟，硫代乙酰胺进行水热反应，离心，固体经过洗涤后真空干燥，得到目标产物。本发明首先通过溶剂热法制备NH2‑UiO‑66晶体，然后在CdIn2S4的合成过程中加入NH2‑UiO‑66，通过水热法使NH2‑UiO‑66与CdIn2S4之间形成异质结，从而得到一种高稳定性、高活性的光催化剂NH2‑UiO‑66/CdIn2S4。该催化剂可以实现在可见光下高效催化水分解制氢。
Description
技术领域
本发明属于催化制氢技术领域，尤其涉及一种NH2-UiO-66/CdIn2S4光催化剂及其制备方法和应用。
背景技术
随着工业化的发展，化石燃料的过度使用造成环境污染，能源短缺等严重问题，给人类社会带来了巨大的伤害，因此清洁能源的开发对于节约能源和保护环境具有重大意义。半导体光催化裂解水制氢是一种最具前景的利用太阳能获取氢能的途径。MOFs材料由于结晶度好，孔隙率高，比表面积大及结构可调控等优点通常被用于光催化。其中，NH2-UiO-66(NU66)由于特殊的热性能及酸性条件下较好的稳定性引起了人们的极大兴趣。然而像许多半导体材料一样，NH2-UiO-66(NU66)的光响应能力较差，光生载流子易复合，因此表现出低光催化活性。近年来，金属硫化物基半导体材料被广泛用于光催化制氢，特别是混合金属硫化物，其可见光响应能力较强，导带电势处于较负的位置，有利于增强可见光的响应能力。在混合金属硫化物中，CdIn2S4(CIS)表现出较好的热稳定性和结构稳定性，因此是最有前景的光催化材料之一。如何获得高活性、高稳定性的催化材料是目前研发的重点，利用不同方法改性的CdIn2S4(CIS)被广泛用于催化领域研究中。
发明内容
本发明的目的是通过水热法将NH2-UiO-66与CdIn2S4复合，得到一种新型材料NH2-UiO-66/CdIn2S4。该材料在催化水分解制氢中具有良好的应用前景。
为实现上述目的，本发明采用的技术方案是：一种NH2-UiO-66/CdIn2S4光催化剂，制备方法包括如下步骤：将NH2-UiO-66晶体溶于去离子水中，然后分别加入2.5水合氯化镉，四水合氯化铟，硫代乙酰胺进行水热反应，离心，固体经过洗涤后真空干燥，得到目标产物。
优选地，上述的NH2-UiO-66/CdIn2S4光催化剂，所述水热反应的条件为180℃加热48h。
优选地，上述的NH2-UiO-66/CdIn2S4光催化剂，按质量之比，NH2-UiO-66：2.5水合氯化镉：四水合氯化铟：硫代乙酰胺＝2：12：31：24。
优选地，上述的NH2-UiO-66/CdIn2S4光催化剂，所述NH2-UiO-66的制备方法为：将适量四氯化锆、2-氨基对苯二甲酸和醋酸加入装有N,N-二甲基甲酰胺的玻璃瓶中，超声均匀，采用溶剂热法，在120℃下反应12h，合成了NH2-UiO-66晶体。
优选地，上述的一种NH2-UiO-66/CdIn2S4光催化剂在光催化水分解制氢中的应用。
优选地，上述的应用，方法如下：将NH2-UiO-66/CdIn2S4光催化剂超声分散于溶有牺牲剂的水溶液中，用Pt作为助催化剂，向溶液中通入氮气除去氧气，在可见光下进行催化反应。
优选地，上述的应用，所述牺牲剂为乳酸。
优选地，上述的应用，所述乳酸浓度为1.2M。
优选地，上述的应用，按固液比，NH2-UiO-66/CdIn2S4光催化剂：含牺牲剂的水溶液＝3mg：10mL。
本发明的有益效果是：本发明利用简单的溶剂热法得到NH2-UiO-66，然后通过水热法将NH2-UiO-66与CdIn2S4复合形成异质结，制备得到了一种具有良好光催化活性的催化剂NH2-UiO-66/CdIn2S4，该催化剂可以实现在可见光下高效催化水分解制氢。
附图说明
图1是CdIn2S4，NH2-UiO-66晶体与NH2-UiO-66/CdIn2S4复合物的固体紫外-可见漫反射光谱图。
图2是NH2-UiO-66/CdIn2S4复合物的扫描电子显微镜图(a)和高分辨透射电子显微镜图(b)。
图3是可见光下(λ≥420nm)NH2-UiO-66/CdIn2S4催化水分解制氢示意图。
图4是可见光下(λ≥420nm)CdIn2S4,NH2-UiO-66,NH2-UiO-66/CdIn2S4催化水分解产氢对比图。
具体实施方式
实施例1
(一)NH2-UiO-66(NU66)晶体的制备方法如下：
将20.4mg四氯化锆(ZrCl4)和14.5mg 2-氨基对苯二甲酸(C8H7NO4)溶于装有10mLDMF(N,N-二甲基甲酰胺)溶液玻璃小瓶中，超声20min。然后，加入1.2mL醋酸(CH3COOH)，密封，在120℃下静置12h。产物经离心分离，然后分别用DMF(N,N-二甲基甲酰胺)和甲醇(CH3OH)反复洗涤，最后80℃真空干燥12h，得到NH2-UiO-66晶体。
(二)CdIn2S4(CIS)的制备方法如下：
分别将114.16mg 2.5水合氯化镉(CdCl2·2.5H2O)，293.17mg四水合氯化铟(InCl3·4H2O)，225.39mg硫代乙酰胺(TAA)加入30mL去离子水中，搅拌30min，然后将溶液转移至50mL反应釜中，在180℃下反应48h。产物经离心分离，然后分别用去离子水和无水乙醇(CH5OH)反复洗涤，最后80℃真空干燥12h，得到纳米球花状的CdIn2S4。
(三)NH2-UiO-66/CdIn2S4(NU66/CIS)的制备方法如下：
将18.8mg NH2-UiO-66晶体加入加入30mL去离子水中，然后分别加入114.16mg2.5水合氯化镉(CdCl2·2.5H2O)，293.17mg四水合氯化铟(InCl3·4H2O)，225.39mg硫代乙酰胺(TAA)，搅拌30min，将溶液转移至50mL反应釜中，在180℃下反应48h。产物经离心分离，然后分别用去离子水和无水乙醇(CH5OH)反复洗涤，最后80℃真空干燥12h，得到NH2-UiO-66/CdIn2S4。
(四)检测结果
图1是CdIn2S4，NH2-UiO-66晶体与NH2-UiO-66/CdIn2S4复合物的固体紫外-可见漫反射光谱图。从图1中可以看出NH2-UiO-66晶体的可见光响应能力较差，而NH2-UiO-66/CdIn2S4表现出较强的可见光响应能力。NH2-UiO-66与CdIn2S4复合后，可见光的吸收范围明显拓宽。
图2是NH2-UiO-66/CdIn2S4复合物的扫描电子显微镜图(a)和高分辨透射电子显微镜图(b)。由图(a)可以看出，CdIn2S4呈纳米球花状结构，NH2-UiO-66呈多面体结构，NH2-UiO-66均匀分散在CdIn2S4表面，并与CdIn2S4紧密结合。如图2中(b)，所测的晶格条纹之间的距离约为0.323nm，对应于CdIn2S4的(311)晶面。
实施例2 NH2-UiO-66/CdIn2S4光催化剂催化水分解制氢
方法如下：该反应在石英反应器中进行，以300W氙灯作为光源模拟太阳光。将催化剂NH2-UiO-66/CdIn2S4(30mg)超声分散于100mL浓度为1.2M乳酸的水溶液中，然后加入400μL0.01mol·L-1的氯铂酸溶液，向反应体系中通入高纯氮气30分钟以除去氧气，然后在可见光(λ≥420nm)照射下反应6h。在反应过程中采用气相色谱法每30分钟检测一次生成氢气的量。参比实验中，分别以CdIn2S4和NH2-UiO-66代替NH2-UiO-66/CdIn2S4作为催化剂。
图3是可见光下(λ≥420nm)NH2-UiO-66/CdIn2S4光催化剂催化水分解制氢示意图。实验结果如图4所示，当NH2-UiO-66作催化剂时，由于其对可见光响应能力较差，因此6h产氢量为零。当CdIn2S4作催化剂时，由于光催化过程中光生电子-空穴对严重复合，6h产氢量仅为87.2μmol·g-1；而NH2-UiO-66/CdIn2S4作催化剂时，催化活性显著提高，产氢量随着反应时间的增加线性上升，反应6h未见活性衰减，6h产氢总量高达683.18μmol·g-1。由此可见，当CdIn2S4与NH2-UiO-66复合形成异质结后，由于电子-空穴对的分离效率提高，光生载流子的迁移速率加快，使CdIn2S4催化水分解放氢活性提高了约7.8倍。NH2-UiO-66/CdIn2S4的催化活性高、稳定性好、制备方法简单，在光催化水分解制氢领域具有良好的应用前景。
Claims (9)
1.一种NH2-UiO-66/CdIn2S4光催化剂，其特征在于，制备方法包括如下步骤：将NH2-UiO-66晶体溶于去离子水中，然后分别加入2.5水合氯化镉，四水合氯化铟，硫代乙酰胺进行水热反应，离心，固体经过洗涤后真空干燥，得到目标产物。
2.根据权利要求1所述的NH2-UiO-66/CdIn2S4光催化剂，其特征在于，所述水热反应的条件为180℃加热48h。
3.根据权利要求1所述的NH2-UiO-66/CdIn2S4光催化剂，其特征在于，按质量之比，NH2-UiO-66：2.5水合氯化镉：四水合氯化铟：硫代乙酰胺＝2：12：31：24。
4.根据权利要求1所述的NH2-UiO-66/CdIn2S4光催化剂，其特征在于，所述NH2-UiO-66的制备方法为：将适量四氯化锆、2-氨基对苯二甲酸和醋酸加入装有N,N-二甲基甲酰胺的玻璃瓶中，超声均匀，采用溶剂热法，在120℃下反应12h，合成了NH2-UiO-66晶体。
5.根据权利要求1所述的一种NH2-UiO-66/CdIn2S4光催化剂在光催化水分解制氢中的应用。
6.根据权利要求5所述的应用，其特征在于，方法如下：将NH2-UiO-66/CdIn2S4光催化剂超声分散于溶有牺牲剂的水溶液中，用Pt作为助催化剂，向溶液中通入氮气除去氧气，在可见光下进行催化反应。
7.根据权利要求6所述的应用，其特征在于，所述牺牲剂为乳酸。
8.根据权利要求7所述的应用，其特征在于，所述乳酸浓度为1.2M。
9.根据权利要求8所述的应用，其特征在于，按固液比，NH2-UiO-66/CdIn2S4光催化剂：含牺牲剂的水溶液＝3mg：10mL。
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| CN116984003A (zh) * | 2023-07-24 | 2023-11-03 | 常州大学 | 一种无牺牲剂析氢的CdIn2S4/MoO3-x复合光催化剂及其制备方法 |
| CN118516691A (zh) * | 2024-07-22 | 2024-08-20 | 浙江石油化工有限公司 | 一种利用波浪能和光能的制氢及降解海水污染物的装置 |
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| CN116984003A (zh) * | 2023-07-24 | 2023-11-03 | 常州大学 | 一种无牺牲剂析氢的CdIn2S4/MoO3-x复合光催化剂及其制备方法 |
| CN118516691A (zh) * | 2024-07-22 | 2024-08-20 | 浙江石油化工有限公司 | 一种利用波浪能和光能的制氢及降解海水污染物的装置 |
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