CN106076371B - 一种AgCl/Ag核壳结构纳米可见光催化剂的制备方法 - Google Patents
一种AgCl/Ag核壳结构纳米可见光催化剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种不对称核壳结构的AgCl/Ag纳米材料的制备方法,所采用的主要技术原理如下:利用壳聚糖只溶于酸性介质的特性将之溶解在含有盐酸的去离子水中,然后加入一定浓度的硝酸银溶液,在壳聚糖大分子的模板作用下形成纳米尺度的AgCl,然后再向体系中引入一定量的α‑氨基丙酸,利用α‑氨基丙酸的还原特性将部分AgCl转化为Ag单质生长在AgCl的表面形成核壳型纳米结构,本发明具有制备方法简便、易得、不需要特殊的设备,更容易推广的优点,且整个制备体系都是由无毒物质组成。
Description
技术领域
本发明涉及一种可见光催化剂的制备方法,具体涉及一种AgCl/Ag核壳结构纳米可见光催化剂的制备方法。
背景技术
全球工业化迅猛发展的同时也带来了日益严重的环境污染,从空气到水体再到土壤无一幸免,因此治理污染成为国内外广泛关注的焦点,也是当前科技领域的研究热点之一。传统的污水治理方法包括物理化学法和生物法两大类,虽然都有一定的效果,但也都不同程度地存在一些缺点。如前者一般处理成本较高、容易形成二次污染等,而后者则对难降解的有机物处理效率不高,因此寻找优异、高效、绿色、低耗的水处理方法是所有环境工作者迫切需要解决的问题。半导体光催化技术是近些年来兴起的一种绿色环境治理技术,被认为是最有前途和最有效的处理方法之一。其中纳米尺度的、能响应太阳光的催化技术最受欢迎,它能够利用太阳能将难降解的有机物完全转化为二氧化碳、水和其他无机小分子,具有高效、清洁、对环境和污染物无特殊要求等特点。而且纳米可见光催化剂不仅可以应用到污水处理方面,还广泛应用于空气净化、土壤修复、杀菌消毒等领域。
最早受到关注的半导体光催化剂是二氧化钛,然而二氧化钛的内禀特性使其投入实际应用存在局限性,如二氧化钛的禁带宽度较大(3~3.2V),仅能对紫外光有吸收,而太阳能到达地球表面后只有4~5%的紫外光,因而对太阳光的利用度非常低。通常使用二氧化钛做催化剂的时候都需要采用高压汞灯之类的专用紫外光源,不仅消耗电能,而且由于紫外线对人体有伤害,对整个光催化设备也有很高要求,从而使得处理量受到限制。相比较而言,具有可见光响应的光催化剂的应用更容易实现,因此,探索新方法制备新形貌的、具有高的光催化活性的可见光催化剂具有重要意义。如现有技术授权公告号:CN101733161B的中国发明专利,该发明实施例提供一种壳聚糖负载金属硫化物光催化剂的制备方法。属于有机无机杂化光催化剂材料制备领域。该方法包括如下步骤:制备壳聚糖金属离子配合物;配制前驱液;光化学反应;光催化剂的后处理:光化学反应结束后,经过滤、洗涤、干燥后即得壳聚糖负载金属硫化物光催化剂。该发明具有制备工艺简单,反应条件温和,反应可控性好、实用性强、设备要求低等优点。所制备的壳聚糖负载金属硫化物光催化剂在紫外光、可见光或自然太阳光下可降解甲基橙、亚甲基蓝等有机物,作为光催化剂在降解有机污染物方面具有较好的应用前景。
发明内容
本发明提供一种制备方法简便、易得、不需要特殊的设备的一种AgCl/Ag核壳结构纳米可见光催化剂的制备方法。
本发明为解决上述问题所采用的技术方案为:
一种AgCl/Ag核壳结构纳米可见光催化剂,该催化剂的核结构为AgCl,壳结构为Ag,利用壳聚糖只溶于酸性介质的特性将之溶解在含有盐酸的去离子水中,加入一定浓度的硝酸银溶液,在壳聚糖大分子的模板作用下形成纳米尺度的AgCl,再向体系中引入一定量的α-氨基丙酸,利用α-氨基丙酸的还原特性将部分AgCl转化为Ag单质生长在AgCl的表面形成核壳型纳米结构。
上述催化剂的核与壳之间以非对称形式复合。
一种AgCl/Ag核壳结构纳米可见光催化剂的制备方法,包括以下步骤:
将浓度为36%的浓盐酸加入去离子水中,并加入壳聚糖搅拌1~2小时使之溶解,然后加入硝酸银,并搅拌均匀后加入还原剂,继续搅拌1小时,得到紫色悬浮液;
将紫色悬浮液静置12小时,所得紫色沉淀离心分离并用去离子水清洗1-5次,即制得AgCl/Ag核壳纳米复合物。
作为优选, 其特征在于:
上述36%的浓盐酸加入去离子水的操作温度为15℃~25℃;
上述壳聚糖搅拌溶解后的浓度为0.5g-1.5g/L;
上述硝酸银加入后,该硝酸银在溶液中的浓度为0.05~0.15 mol•L-1;
上述还原剂加入后,该还原剂在溶液中浓度为0.05~0.15 mol•L-1。
作为优选,上述的还原剂为α-氨基丙酸,是一种氨基酸,从而使得所制备的光催化剂完全生物相容,可以应用到饮用水净化和与人类生活密切相关环境的空气净化等领域。
作为优选,上述所得紫色沉淀离心分离并用去离子水清洗2次。
与已有技术相比,本发明具有如下优点:
1、所得到的AgCl /Ag纳米复合光催化剂对阴面房间的散射光具有响应,能够完成对模型有机物的完全降解;
2、整个制备体系都是由无毒物质组成的,特别是壳聚糖是一种生物相容性良好的物质,其本身就来源于甲壳类动物的壳,而α-氨基丙酸是一种氨基酸,从而使得所制备的这种光催化剂完全生物相容,可以应用到饮用水净化和与人类生活密切相关环境的空气净化等领域;
3、制备方法简便、易得、不需要特殊的设备,更容易推广。
附图说明
图1实施例1的AgCl /Ag纳米核壳结构的透射电子显微镜镜图像;
图2实施例2的AgCl /Ag纳米核壳结构的透射电子显微镜镜图像;
图3模型染料(罗丹明B)和与AgCl /Ag纳米核壳光催化剂混合并置于阴面房间三天后的数码图像;
图4模型染料(亚甲基蓝)和与AgCl /Ag纳米核壳光催化剂混合并置于阴面房间三天后的数码图像。
具体实施例
下面结合附图和具体实施例对本发明做进一步的说明,但本发明的制备方案不受限于这些实施例。
实施例:
(1)将1 mL的浓盐酸加到20 mL去离子水中,加入0.2 g的壳聚糖并搅拌1小时使之完全溶解,所述浓盐酸浓度为36%;
(2)加入硝酸银,使其浓度为0.1 mol•L-1, 搅拌均匀后加入α-氨基丙酸,使其浓度为0.2 mol•L-1;
(3)继续搅拌1小时后,将反应体系静置12小时,将所得紫色沉淀离心分离并用去离子水清洗两次留用。这些紫色沉淀通过透射电子显微镜表征可以看到明显的非对称核壳结构,如图1。
(4)所有步骤都在环境温度下完成,环境温度为15℃~25℃下。
实施例2:
(1)将1.5 mL的浓盐酸加到20 mL去离子水中,加入0.3 g的壳聚糖并搅拌2小时使之完全溶解,所述浓盐酸浓度为36%;
(2)加入硝酸银,使其浓度为0.15 mol•L-1, 搅拌均匀后加入α-氨基丙酸,使其浓度为0.3 mol•L-1;
(3)继续搅拌1小时后,将反应体系静置12小时,用吸管吸去上层清液,再加入20mL的去离子水,搅拌5分钟后继续静置并重复上述操作2次以实现对产物的清洗。将所得紫色沉淀离心分离并用去离子水清洗两次留用。这些紫色产物形貌通过透射电子显微镜表征,可以看到明显的核壳结构,如图2。
(4)所有步骤都在环境温度下完成,环境温度为15℃~25℃下。
核壳型AgCl/Ag复合纳米材料光催化剂的性能研究
取适量步骤一所制得的AgCl/Ag复合纳米光催化剂超声分散在浓度为20 mg•L-1的模型染料水溶液中,于暗处搅拌0.5小时达到吸附平衡后,在不同可见光源辐照下开始光催化性能研究实验,这些光源包括:氙灯、家用日光灯和自然光,自然光可以是太阳光直接照射,也可以是阴面房间里自然光的散射光。每隔一定时间间隔取约三毫升左右的催化体系液体离心分离,取上层清液通过紫外可见分光光谱仪分析模型染料的特征峰吸光度值来判断光催化的进程直至染料完全降解,完全脱色所需时间与光强度有关。模型染料可以是亚甲基兰、罗丹明B、甲基橙、甲基紫等多种,除模型染料外,被降解的物质还可以是其他有机污染物,如硝基苯等。典型示例见图3。
对比实验:
实验方法:设置实验组A和对照组B,其中实验组为本实施例所的产品,分别对其特征和降解做记录,结果如下表1。
模型染料 | 有机污染物 | 降解速度 | 对环境的影响 | |
实验组A | 优 | 优 | 优 | 优 |
对照组B | 良 | 优 | 良 | 优 |
从上表可以看出,实验组在模型染料、降解速度、明显优与对照组,且可以看出本实施例所得产品在降解模型染料方面具有较好的应用前景,降解速度优于试验组,可以更好的减少降解周期。
虽然本发明已以实施例公开如上,但其并非用以限定本发明的保护范围,任何熟悉本领域的技术人员,在不脱离本发明的构思和范围内所做的更动和润饰,均应属于本发明所附权利要求的保护范围。
Claims (3)
1.一种AgCl/Ag核壳结构纳米可见光催化剂的制备方法,其特征在于以下步骤:
1)将浓度为36%的浓盐酸加入去离子水中,并加入壳聚糖搅拌1~2小时使之溶解,然后加入硝酸银,并搅拌均匀后加入还原剂,继续搅拌1小时,得到紫色悬浮液;
2)将紫色悬浮液静置12小时,所得紫色沉淀离心分离并用去离子水清洗1-5次,即制得AgCl/Ag核壳纳米复合物;
所述的步骤1)中还原剂为α-氨基丙酸;
所述的硝酸银的浓度为0.15mol·L-1,α-氨基丙酸的浓度为0.3mol·L-1;
所述的壳聚糖搅拌溶解后的浓度为0.5g-1.5g/L。
2.根据权利要求1所述的制备方法,其特征在于:
所述的步骤1)中:
所述的36%的浓盐酸加入去离子水的操作温度为15℃~25℃。
3.根据权利要求1所述的制备方法,其特征在于:步骤2)所述的去离子水清洗为2次。
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CN103302307A (zh) * | 2013-06-25 | 2013-09-18 | 通化师范学院 | 一种银纳米粒子的制备方法及其促进黄瓜种子萌发、幼苗生长发育的方法 |
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