CN107413358B - 一种黑磷量子点/凹凸棒纳米复合材料及其制备方法和应用 - Google Patents
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Abstract
本发明属于化工新材料领域,特别涉及一种黑磷量子点/凹凸棒纳米复合材料及其制备方法和应用。将黑磷粉末、凹凸棒和NaOH分散于有机溶剂中,并在惰性气体保护下进行溶剂热搅拌反应,反应结束后经过高速离心取上层悬浮液真空烘干得到黑磷量子点/凹凸棒纳米复合材料;将该纳米复合材料用于脱硝,与传统的SCR脱硝相比,低温下对NO的转化效率明显提高,可大大降低能耗。
Description
技术领域
本发明属于化工新材料领域,特别涉及一种黑磷量子点/凹凸棒纳米复合材料及其制备方法和应用。
背景技术
作为纳米材料家族中的重要一员,纳米量子点材料以其量子隧道效应、丰富活性位、上转换荧光、优异电子传输等特性引起了人们的极大关注,在光电子器件、催化、生物荧光标记等领域展示了巨大的应用前景。
其中,黑磷量子点作为近两年刚刚涌现出来的新型量子点材料正越来越吸引人们的兴趣,它往往由它的母体--黑磷单晶或粉末逐步解离而得来,由于黑磷量子点对空气和水非常敏感,常常需要惰性气体隔绝保护,且制备过程均较为苛刻,而且只能得到有机溶剂溶液态的单一黑磷量子点,很大程度上限制了黑磷量子点的功能化应用前景。
发明内容
本发明旨在提供一种黑磷量子点/凹凸棒纳米复合材料及其制备方法和应用,即遴选合适的原料及工艺流程得到稳定的黑磷量子点/凹凸棒光催化材料,并将其用于尾气脱硝,
本发明的黑磷量子点/凹凸棒纳米复合材料是以凹凸棒为载体,将凹凸棒与黑磷量子点复合后得到的纳米材料,组成通式表示为BPQD/ATP。
上述黑磷量子点/凹凸棒纳米复合材料的制备方法为:将黑磷粉末、凹凸棒和NaOH分散于有机溶剂中,并在惰性气体保护下进行溶剂热搅拌反应,反应结束后经过高速离心取上层悬浮液真空烘干得到黑磷量子点/凹凸棒纳米复合材料,
其中,有机溶剂为n-甲基-2-吡咯烷酮,
惰性气体为氮气,氦气或氩气,
溶剂热搅拌反应具体为,于120~180℃下剧烈搅拌反应4~10h。
本发明的有益效果在于:本发明采用溶剂热法制备得到黑磷量子点/凹凸棒纳米复合材料,避免了传统制备工艺中的机械剥离,所得黑磷量子点粒径小于5nm,分散均匀,而且发挥了凹凸棒保护黑磷量子点产品不受空气氧化的优势(这可能是基于凹凸棒表面丰富的活性位以及形成的Si-O-P化学键等多方面的协同作用);
本发明中黑磷量子点被可见光激发后产生光生电子与空穴,与NH3协同作用共同将NO在室温下即可还原为N2,大大降低了能耗。具体为:空穴与NH3产生·NH2自由基,再与NO生成NH2NO中间产物,最后分解为氮气和水。
附图说明
图1为实施例1制备的黑磷量子点/凹凸棒纳米复合材料的SEM图。
图2为实施例1制备的黑磷量子点/凹凸棒纳米复合材料的TEM图。
具体实施方式
实施例1
将0.35g黑磷粉末、1.0g凹凸棒和0.2gNaOH分散于100ml n-甲基-2-吡咯烷酮中,并在氮气保护下于120℃下剧烈搅拌10小时,反应结束后经过7000rpm高速离心2h,取上层悬浮液真空烘干得到黑磷量子点/凹凸棒纳米复合材料,对所得产品进行扫描电镜和透射电镜观察,SEM和TEM图分别如图1和图2所示:凹凸棒呈现纳米棒状结构,黑磷量子点大小均一,均匀地负载在凹凸棒上。
实施例1中的黑磷量子点/凹凸棒纳米复合材料制备完成后即刻用于光催化脱硝,具体操作为:在脱硝装置石英管中加入5mL该黑磷量子点/凹凸棒纳米复合材料,反应气体配比均为:0.1%(相对于气体总流量的体积百分比,下同)NH3、0.1%NO以及3%的O2,N2作为平衡气,气体总流量控制在1.5L/min,所使用的光源为500W的氙灯,脱硝在常温(25℃)下进行。通过烟气检测仪检测入口NO浓度和出口NO浓度,测得复合材料对NO的转化率达95%;
将实施例1制备的黑磷量子点/凹凸棒纳米复合材料于空气气氛中常温(25℃,下同)放置3天后用于光催化脱硝,具体操作同上。通过烟气检测仪检测入口NO浓度和出口NO浓度,测得复合材料对NO的转化率达93.7%。
对比实施例1
采用石墨烯作为载体代替实施例1中的“凹凸棒”,其余操作均同实施例1。
按照实施例1中的脱硝操作:
本对比实施例中的黑磷量子点/石墨烯复合材料制备完成后即刻用于光催化脱硝,对NO的转化率为85%;
将本对比实施例中得到的黑磷量子点/石墨烯复合材料于空气气氛中常温放置3天后用于光催化脱硝,对NO的转化率仅为65.6%。
对比实施例2
采用蒙脱土作为载体代替实施例1中的“凹凸棒”,其余操作均同实施例1。
按照实施例1中的脱硝操作:
本对比实施例中的黑磷量子点/蒙脱土复合材料制备完成后即刻用于光催化脱硝,对NO的转化率为73.2%;
将本对比实施例中得到的黑磷量子点/蒙脱土复合材料于空气气氛中常温放置3天后用于光催化脱硝,对NO的转化率仅为48%。
从对比实施例1和2中看出,黑磷量子点复合材料于空气中放置一定时间后光催化效果明显下降,这主要是基于空气对复合材料中的有效成分黑磷量子点的氧化所导致;而实施例1的方案中采用凹凸棒作为载体时,却很好地避免了这一风险。
实施例2
将0.32g黑磷粉末、0.8g凹凸棒和0.3gNaOH分散于100ml n-甲基-2-吡咯烷酮中,并在氩气保护下于140℃下剧烈搅拌8小时,反应结束后经过7000rpm高速离心2h,取上层悬浮液真空烘干得到黑磷量子点/凹凸棒纳米复合材料,后续检测如实施例1。
实施例3
将0.28g黑磷粉末、1.0g凹凸棒和0.3gNaOH分散于100ml n-甲基-2-吡咯烷酮中,并在氮气保护下于160℃下剧烈搅拌6小时,反应结束后经过7000rpm高速离心2h,取上层悬浮液真空烘干得到黑磷量子点/凹凸棒纳米复合材料,后续检测如实施例1。
实施例4
将0.36g黑磷粉末、1.0g凹凸棒和0.5gNaOH分散于100ml n-甲基-2-吡咯烷酮中,并在氮气保护下于150℃下剧烈搅拌7小时,反应结束后经过7000rpm高速离心2h,取上层悬浮液真空烘干得到黑磷量子点/凹凸棒纳米复合材料,后续检测如实施例1。
实施例5
将0.28g黑磷粉末、1.0g凹凸棒和0.4gNaOH分散于100ml n-甲基-2-吡咯烷酮中,并在氮气保护下于180℃下剧烈搅拌4小时,反应结束后经过7000rpm高速离心2h,取上层悬浮液真空烘干得到黑磷量子点/凹凸棒纳米复合材料,后续检测如实施例1。
Claims (5)
1.一种黑磷量子点/凹凸棒纳米复合材料的制备方法,其特征在于:所述的复合材料为,以凹凸棒为载体,将凹凸棒与黑磷量子点复合后得到的纳米材料;
制备方法为:将黑磷粉末、凹凸棒和NaOH分散于有机溶剂中,并在惰性气体保护下进行溶剂热搅拌反应,反应结束后经过高速离心取上层悬浮液真空烘干得到黑磷量子点/凹凸棒纳米复合材料。
2.如权利要求1所述的黑磷量子点/凹凸棒纳米复合材料的制备方法,其特征在于:所述的有机溶剂为n-甲基-2-吡咯烷酮。
3.如权利要求1所述的黑磷量子点/凹凸棒纳米复合材料的制备方法,其特征在于:所述的惰性气体为氦气或氩气。
4.如权利要求1所述的黑磷量子点/凹凸棒纳米复合材料的制备方法,其特征在于:所述的溶剂热搅拌反应具体为,于120~180℃下剧烈搅拌反应4~10h。
5.一种如权利要求1所述的方法制备黑磷量子点/凹凸棒纳米复合材料的应用,其特征在于:所述的应用为,将所述纳米复合材料用于脱硝。
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