CN106115766B - 一种高效降解染料的纳米材料的制备方法 - Google Patents
一种高效降解染料的纳米材料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种高效降解染料的纳米材料的制备方法,其氧化锌纳米片的制备为:首先将二水合醋酸锌加入到无水乙醇中并加入螯合剂乙醇胺和聚乙二醇,搅拌获得透明稳定的氧化锌溶胶,然后将实验室常用的滤纸模板浸渍到氧化锌溶胶中,最后焙烧除去滤纸和其他有机物质得到氧化锌纳米片,所制备的氧化锌纳米片物相为JCPDS 编号为65‑3411的六方纤锌矿结构氧化锌,形状为片状,片层厚度~80nm。本发明制备方法简便,产出率高,所用滤纸模板绿色环保、成本低廉,得到的氧化锌纳米片在光照下对甲基橙表现出良好的降解活性,反应60min时甲基橙降解率达到90%以上。
Description
本发明是申请号为2014106857865、申请日2014年11月25日的发明专利的分案申请。
技术领域
本发明属于无机纳米材料技术领域,尤其涉及一种氧化锌纳米材料的制备方法。
背景技术
印染行业中甲基橙等大量水溶性偶氮染料的大量排放,使人类赖以生存的水质日益恶化。这些污染物质多难生物降解,一旦进入水体,由于其在水体中自然降解过程缓慢,其危害性延滞较长。光催化反应可以将污染物在光照条件下完全矿化为各种无机离子,因此在环境治理方面得到了广泛关注,关于光催化剂的研发,成为目前国内外的研究热点。
在光催化领域,纳米氧化锌作为催化剂时能使水中的有害有机物质最终分解,避免其对环境的污染。研究表明,纳米氧化锌的反应速度是大块氧化锌材料的100~1000倍,而且与普通粒子相比,纳米氧化锌几乎不会引起光的散射,因此是极具应用前景的光催化剂之一。到目前为止,人们已经用化学气相沉积法,共沉淀法,溶胶凝胶法,水热法等多种方法制备出了不同形貌的纳米氧化锌。虽然制备方法很多,但仍都存在一些不足,目前制备得到的氧化锌对污染物的降解效率仍待提高。寻求价廉、环境友好并具有高催化活性的光催化材料是光催化技术发展的关键。
发明内容
本发明的目的在于提供一种高效降解染料的纳米材料的制备方法。
本发明目的通过如下技术方案实现:
本发明提供的方法是使用廉价的实验室常用滤纸为模板,将氧化锌凝胶包覆在滤纸表面,最后除去滤纸,得到在光照条件下对染料甲基橙的降解具有高效催化效果的氧化锌纳米片。具体包括以下步骤:
1)配置0.3~0.8mol/L的醋酸锌[Zn(CH3COO)2•2H2O]溶液,一定温度下搅拌至溶液呈乳浊液;所述反应在65-75℃水浴中进行;
2)向上述乳浊液中逐滴加入乙醇胺(DEA),搅拌一段时间至溶液变澄清后再加入一定量聚乙二醇(PEG)并持续搅拌直至获得透明稳定的氧化锌溶胶体系;
3)将实验室常用定量无灰滤纸浸渍到上述溶胶溶液中,浸泡1~3h;
4)收集滤纸,使用无水乙醇洗涤干燥后,放入管式炉焙烧,焙烧过程采用分段焙烧法,首先将样品加热至100℃保温1h,然后继续升温至500℃焙烧3h,郑个升温过程保持2℃/min的加热速率,焙烧完毕后自然炉冷至室温,得到氧化锌纳米片。
上述整个制备过程保持无水状态。
本发明具有如下有益效果:
本发明方法使用实验室常用无灰定量滤纸作为氧化锌纳米片的模板,原料绿色环保,简单易得,成本低廉,整个实验过程过程简单,操作方便,很容易实现产物的大规模生产,所制备的氧化锌纳米片物相为JCPDS 编号为65-3411的六方纤锌矿结构氧化锌,形状为片状,片层厚度~80nm。得到的氧化锌纳米片在光照下对甲基橙表现出良好的降解活性,反应60min时甲基橙降解率达到90%以上,在污水处理方面具有广阔的应用前景。
附图说明
图1 是制备的氧化锌纳米片的XRD图。
图2 是制备的氧化锌纳米片的SEM图。
图3 是制备的氧化锌纳米片的TEM图。
图4是制备的氧化锌纳米片对甲基橙降解反应的光催化效果图。
具体实施方式
下面结合实施例对本发明进行进一步说明。本发明的生产技术对本专业的人来说是容易实施的。本实施例在以本发明技术方案为前提下进行实施,给出了详细的实施方式和过程,但本发明的保护范围不限于下述的实施例。
实施例1
70℃下水浴条件下,将6.58g的醋酸锌[Zn(CH3COO)2•2H2O]加入到50mL的无水乙醇中,搅拌30min得到氧化锌乳浊液。
搅拌条件下,向上述溶液中逐滴加入3.154g乙醇胺(DEA),搅拌一段时间至乳浊液变澄清时,再加入0.7g的聚乙二醇(PEG)并持续搅拌2h,直至获得透明稳定的氧化锌溶胶。
将预先剪好的5mm×5mm 大小的150mg实验室常用无灰定量滤纸投入到上述氧化锌溶胶中,浸泡3h。
将上述浸泡过的滤纸用无水乙醇洗涤数次后,置于真空干燥箱中干燥过夜,最后放入管式炉中以2℃/min的加热速率首先加热至100℃保温1h,然后继续升温至500℃焙烧3h。
材料的光催化性能测试:
准确称量0.2 g 的氧化锌纳米材料加入500 ml甲基橙溶液(25 mg/L)中,超声分散;所得悬浮液避光搅拌1 h 使材料达到吸附平衡;平衡后取出3 ml 悬浮液,将剩余悬浮液倒入500 ml 石英管中,然后放入光催化反应仪中;开启500 W 汞灯照射,每隔20 min取3ml 悬浮液于离心管中,总反应时间2h ;反应结束,取出的各个样品经离心分离后,取上清液用紫外-可见分光光度计测其在460 nm 左右的吸光度,从而反映各个降解时间段后剩余甲基橙的浓度,以此来反映本方法制得氧化锌光催化剂降解甲基橙的效果。
Claims (1)
1.一种高效降解染料甲基橙的纳米材料的制备方法,其特征在于,步骤如下:
(1)、70℃下水浴条件下,将6.58g的醋酸锌[Zn(CH3COO)2•2H2O]加入到50mL的无水乙醇中,搅拌30min得到氧化锌乳浊液;
(2)、搅拌条件下,向上述溶液逐滴加入3.154g乙醇胺(DEA),搅拌至乳浊液变澄清时,再加入0.7g的聚乙二醇(PEG)并持续搅拌2h,直至获得透明稳定的氧化锌溶胶;
(3)、将预先剪好的5mm×5mm 大小的150mg无灰定量滤纸投入到上述氧化锌溶胶中,浸泡3h;
(4)、将上述浸泡过的滤纸用无水乙醇洗涤后,置于真空干燥箱中干燥过夜,最后放入管式炉中以2℃/min的加热速率首先加热至100℃保温1h,然后继续升温至500℃焙烧3h。
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