CN104944369B - 一种银修饰钽酸钠等离子催化剂分解水制氢的方法 - Google Patents

一种银修饰钽酸钠等离子催化剂分解水制氢的方法 Download PDF

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CN104944369B
CN104944369B CN201410722439.5A CN201410722439A CN104944369B CN 104944369 B CN104944369 B CN 104944369B CN 201410722439 A CN201410722439 A CN 201410722439A CN 104944369 B CN104944369 B CN 104944369B
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sodium tantalate
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CN104944369A (zh
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施伟东
徐东波
罗必富
李萍
陈敏
范伟强
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Jiangsu University
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Abstract

本发明涉及一种以硝酸银和钽酸钠为原料制备银修饰钽酸钠等离子体催化剂分解水制氢的方法。取钽酸钠和硝酸银加入到水和甲醇的混合溶剂中，硝酸银与钽酸钠质量之比为0.0008‑0.0032：1，然后放到氙灯下面，磁力搅拌使反应液混合均匀，打开光源分解水制氢，反应结束后，将沉淀过滤，洗涤，烘干得到所述的等离子体催化剂。

Description

一种银修饰钽酸钠等离子催化剂分解水制氢的方法
技术领域
本发明涉及一种以硝酸银和钽酸钠为原料制备银修饰钽酸钠等离子体催化剂分解水制氢的方法，尤其是一种制备工艺简单，具有良好光催化活性分解水制氢的纳米复合光催化剂。
技术背景
纳米粒子由于特殊的物理和化学性质，在物理、化学、材料科学以及生物医学领域受到了广泛的关注，其中研究最为广泛的就是银纳米粒子；银纳米粒子具有独特的光学和催化性质，而且无毒性，具有生物亲和性，使其在生物传感、化学催化、电子元件以及生物医药等领域都有广泛的应用前景，因而，一些研究者利用金属银负载在纳米半导体化合物表面，构筑出具有等离子体共振效应的复合体系，这一体系具有高效利用可见光的作用；JunFang等人（International journal of hydrogen energy 2012, 37, 17853.）制备出金负载在纳米二氧化钛表面，Nelson, J. A.等人（J. Am. Chem. Soc. 2003, 125, 332.）制备出银负载在氯化银表面，这种利用等离子体构筑复合光催化剂应用很广。
碱土金属钽酸钠（NaTaO3）的导带由Ta5d轨道构成，远远高于Ti3d轨道，因此与二氧化钛（TiO2）相比，光激发钽酸钠产生的电子具有更强的还原能力，更有利于实现高效光催化分解有机物；目前，Xia Li 等人（J. Phys. Chem. C 2009,113,19411–19418.）研究了利用水热法合成钽酸钠在不同时间和温度、不同氢氧化钠与五氧化二钽配比的情况下的形貌变化，最后制备出立方体的钽酸钠，并验证在紫外光下分解亚甲基蓝的效果，因而，我们构筑一种银修饰钽酸钠等离子体催化剂在分解水制氢方面的应用。
发明内容
本发明目的是提供一种以硝酸银和钽酸钠为原料，合成具有良好光催化活性的纳米复合等离子体光催化剂分解水制氢的方法。
本发明通过以下步骤实现：
（1）取钽酸钠和硝酸银加入到水和甲醇的混合溶剂中，硝酸银与钽酸钠质量之比为0.0008-0.0032：1，然后放到氙灯下面，磁力搅拌使反应液混合均匀，打开光源分解水制氢，反应结束后，将沉淀过滤，洗涤，烘干得到所述的等离子体催化剂。
所述水和甲醇的混合溶剂中，水和甲醇的体积比为3:1。
本发明中所使用的氙灯为 300 W。
本发明中所使用氙灯照射时间为 5 h。
本发明所得银修饰钽酸钠等离子体复合光催化剂，晶化完全，银微粒粒径小于10nm，形貌规则，分散性良好。
利用透射电子显微镜（TEM）、高分辨投射电子显微镜（HRTEM）、X光电子能谱仪等仪器对产物进行形貌结构分析。
在分解水制氢过程中，银离子首先受到光照被还原成银纳米粒子附着在钽酸钠表面，继续光照，银纳米粒子上的电子被激发与水中的氢离子结合生成氢气，钽酸钠上的电子传输到银纳米粒子表面，剩下空穴，氧化甲醇，从而形成一个持续的氧化还原过程，银纳米粒子的存在加速了电子的转移，因而产氢速率相比纯钽酸钠有所提高。
附图说明
图1为所制备不同质量的银修饰钽酸钠等离子体复合光催化剂的透射电镜照片；其中钽酸钠200mg，a为0.16mg的硝酸银，b为0.32mg的硝酸银，c为0.64mg的硝酸银。
图2为所制备银修饰钽酸钠等离子体复合光催化剂的能量色散X射线谱图。
图3为所制备银修饰钽酸钠等离子体复合光催化剂的高分辨透射电镜照片。
图4为所制备银修饰钽酸钠等离子体复合光催化剂的高分辨透射电镜mapping照片。
图5为在合成不同质量的银修饰钽酸钠等离子体复合光催化剂的过程中分解水制氢的时间-速率柱状图；其中钽酸钠200mg，a为不加硝酸银，b为0.16mg的硝酸银，c为0.32mg的硝酸银，d为0.64mg的硝酸银。
具体实施方式
实施例1 不同质量的银修饰钽酸钠等离子体复合光催化剂的分解水制氢实验
（1）将150mL去离子水和50mL甲醇配成溶液。
（2）分别称取硝酸银0.16mg(0.08wt%)，0.32mg(0.16wt%),0.64mg(0.32wt%)和200mg钽酸钠，分别置于含有上述溶液的光催化反应器中，磁力搅拌，待复合光催化剂分散均匀后，打开水源，光源，进行光催化分解水制氢实验。
（3）每5 h测量氢气的产量。
（4）由图5可见银修饰钽酸钠等离子体复合光催化剂具有优异的光催化分解水制氢活性，尤其是硝酸银的质量为0.32 mg(0.16wt%)的样品，比纯的钽酸钠分解水制氢活性大约高2倍。
实施例2 银修饰钽酸钠等离子体复合光催化剂获得
分解水制氢测试反应结束后，过滤得产物用去离子水洗净，恒温干燥箱中60 ℃烘干，即为银修饰钽酸钠等离子体复合催化剂。
实施例3 银修饰钽酸钠等离子体复合光催化剂表征分析
如图1所示，图中可以清楚看到银原子的存在。
如图2所示，图谱中显示出银的特征峰。
如图3所示，图中可以清楚看到银纳米粒子小于10nm。
如图4所示，图中可以清楚看到银纳米粒子均匀的分布。

Claims (4)

1.一种银修饰钽酸钠等离子体催化剂分解水制氢的方法，其特征在于：取钽酸钠和硝酸银加入到水和甲醇的混合溶剂中，硝酸银与钽酸钠质量之比为0.0016：1，然后放到氙灯下面，磁力搅拌使反应液混合均匀，打开光源分解水制氢，所使用的氙灯为300W，反应结束后，将沉淀过滤，洗涤，烘干得到银修饰钽酸钠等离子体复合光催化剂；在分解水制氢过程中，银离子首先受到光照被还原成银纳米粒子附着在钽酸钠表面，继续光照，银纳米粒子上的电子被激发与水中的氢离子结合生成氢气，钽酸钠上的电子传输到银纳米粒子表面，剩下空穴，氧化甲醇，从而形成一个持续的氧化还原过程，银纳米粒子的存在加速了电子的转移，产氢速率相比纯钽酸钠有所提高。
2.如权利要求1所述的一种银修饰钽酸钠等离子体催化剂分解水制氢的方法，其特征在于：所述水和甲醇的混合溶剂中，水和甲醇的体积比为3:1。
3.如权利要求1所述的一种银修饰钽酸钠等离子体催化剂分解水制氢的方法，其特征在于：所述氙灯照射时间为5h。
4.如权利要求1所述的一种银修饰钽酸钠等离子体催化剂分解水制氢的方法，其特征在于：所述银修饰钽酸钠等离子体复合光催化剂，晶化完全，银微粒粒径小于10nm，形貌规则，分散性良好。
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