CN114054016B - 一种多孔氧化铌纳米材料及其制备方法和在碳中和中的应用 - Google Patents
一种多孔氧化铌纳米材料及其制备方法和在碳中和中的应用 Download PDFInfo
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Abstract
本发明公开了一种多孔氧化铌纳米材料及其制备方法和在碳中和中的应用,属于无机非金属材料制备、环境保护技术和太阳能利用技术领域。该多孔氧化铌材料通过可分解模板法来获得,在结晶成相过程伴随着模板的分解,限制晶粒之间的熟化,成功获得具有多孔微观结构的纳米材料。所述多孔氧化铌纳米材料在太阳光照射下具有良好的有机物降解性能和二氧化碳还原性能,可以直接应用于解决水中有机污染物的光催化降解和二氧化碳的资源化转化。
Description
技术领域
本发明属于无机非金属纳米材料制备、太阳能利用和二氧化碳转化利用技术领域,具体为一种多孔氧化铌纳米材料及其制备方法和在碳中和中的应用。
背景技术
能源危机及环境污染是当今时代人类所面临的两大难题,光催化技术因为能有效利用太阳能,几乎可以将任何有机分子氧化,矿化为二氧化碳和无机离子,在降解水中的有机污染物,杀灭水中细菌、病毒等微生物方面受到人们的广泛关注。在众多的光催化剂中,一些宽禁带的n型半导体如二氧化钛、氧化锌、氧化锡等因低毒、廉价、稳定性高和环境友好型等特点被广泛的应用于光解水制氢、太阳能电池和环境修复等领域。
如何更加有效地转化污染物(或者是目标物),是提高太阳能利用率的一个重要方向,同时也是光催化剂设计的一个热点研究方向。其中,提高光催化材料的表面活性,以提高材料与污染物之间电荷转移效率,被认为是提高光催化反应效率一个重要的思路。
对于常见的氧化物半导体来说,以氧化铌为例,其具有较高的导带,光照下激发的光生电子具有较高的能量,可以用来还原环境中的目标物,有望应用于环境修复以及二氧化碳转化领域。要获得晶化良好的材料体系就必不可少地要引入加热或者是煅烧的工艺。但是该工艺的引入又会带来光催化材料晶粒的长大,减少材料表面的活性位点,从而降低了氧化物半导体的光催化活性。这种表面活性位点的降低对于光催化转化气体分子是十分不利的。因此,为了便于工业化推广以及提高光催化材料表面活性的考虑,开发一种简单可行的改进煅烧制备工艺,在尽可能地保留光催化材料表面活性位点的前提下提高氧化物的晶化程度以促进光生电子与空穴的分离,是环境修复材料领域以及太阳能利用领域一个重要的研究方向。
发明内容
本发明的目的在于提供一种多孔氧化铌纳米材料及其制备方法和在碳中和中的应用,所述多孔氧化铌材料通过可分解模板法来获得,在结晶成相过程伴随着模板的分解,限制晶粒之间的熟化,成功获得具有多孔微观结构的纳米材料。所述多孔氧化铌纳米材料在太阳光照射下具有良好的有机染料降解性能和二氧化碳还原性能,可以直接应用于解决水中有机污染物的光催化降解和二氧化碳的资源化转化。
为实现上述目的,本发明所采用的技术方案是:
一种多孔氧化铌纳米材料,其为六方晶体结构,晶粒尺寸为5-50nm,具有纳米孔的微观结构。
所述的多孔氧化铌纳米材料是通过前驱体配制—模板热解—洗涤干燥的工艺流程制备获得的,其制备方法具体包括如下步骤:
(1)前驱体配制:首先配置1-1000mmol/L的铌盐溶液,随之将其缓慢滴入碳酸铵固体粉末中,获得模板热解的混合体系;
(2)模板热解:将步骤(1)获得的混合体系,置于300~600℃温度下保温0.5-20h;
(3)洗涤干燥:将经步骤(2)模板热解后所得粉末,用二次去离子水和无水乙醇交替洗涤5~8次,放入干燥箱在40~120℃温度下干燥一天,即得到所述多孔氧化铌纳米材料。
上述步骤(1)中,用于配制铌盐溶液的溶剂为水、酒精和乙二醇中的一种或几种混合,铌盐为氯化铌、乙酸铌或硝酸铌酰。
步骤(1)中,所述铌盐溶液中的铌盐与碳酸铵固体粉末的重量比例为1:(10-50)。
将所述多孔氧化铌纳米材料直接应用于有机染料的光催化降解;或者将所述多孔氧化铌纳米材料直接应用于二氧化碳的光催化转化,可将二氧化碳转化为烯烃。
本发明的设计原理如下:
本发明首先配置一定浓度的铌盐溶液,然后将其缓慢滴加进入到碳酸铵粉末体系中,该过程使得铌离子产生氧化物的前驱体,同时大量碳酸铵粉末的存在可以作为一种硬模板,更好地分散铌离子,从而在空间上限制了氧化铌的长大。通过对上述前驱体体系进行简单的煅烧,即可获得具有微观多孔结构的氧化铌纳米材料,该氧化铌纳米材料具有细小的晶粒以及丰富的表面活性位点,能够为光催化反应产生足够的表面位点,从而提高了光催化反应的效率。
本发明的优点在于:
1.本发明通过用可分解硬模板法进行氧化铌纳米材料的制备,克服了常规固相法制备氧化铌时易发生团聚的缺点。
2.本发明通过微观多孔结构的引入,提高了氧化铌材料的表面活性。
3.本发明的氧化铌纳米材料实现了将二氧化碳转化为有用的烯烃。
4.本发明的氧化铌纳米材料能直接应用于太阳光下有机污染物的净化降解。
5.本发明采用简单的煅烧工艺来制备多孔的氧化铌纳米材料,大大降低了材料制备过程中的设备要求,适合工业化的推广。
附图说明:
图1为本发明氧化铌纳米材料X射线衍射图谱。
图2为本发明氧化铌纳米材料的透射电镜照片。
图3为本发明氧化铌纳米材料对于水溶液中罗丹明B的降解曲线。
图4为本发明氧化铌纳米材料对于二氧化碳的光催化转化性能。
具体实施方式:
以下通过附图及实施例详述本发明。
实施例1
本实施例的工艺流程为:通过前驱体配制—模板热解—洗涤干燥的工艺流程获得氧化铌纳米材料。具体如下:
首先配置100mmol/L的铌盐溶液,随之将其缓慢滴入碳酸铵固体粉末中(铌盐和碳酸铵固体粉末的质量比为1:20),获得模板热解的混合体系;将所获得的混合体系,置于550℃温度下保温2h;将煅烧后所得粉末,用二次去离子水和无水乙醇交替洗涤8次,放入干燥箱在60℃温度下干燥一天。
对比例1
本对比例的工艺流程为:通过沉淀干燥+煅烧的工艺流程获得氧化铌材料。
具体如下:
首先取少量pH=13的浓氨水,用去离子水稀释至pH=9.2。取75毫升铌盐溶液中,缓慢滴加至75毫升稀释后的氨水溶液;去掉混合体系中上清残液,将剩余沉淀用二次去离子水和无水乙醇交替洗涤8次,放入干燥箱在60℃温度下干燥一天;将干燥后的沉淀研磨至细粉状,置于550℃温度下保温2h。将煅烧后所得粉末,用二次去离子水和无水乙醇交替洗涤5~8次,放入干燥箱在40~120℃温度下干燥一天。
实施例2
将实施例1和对比例1所得氧化铌纳米材料用于罗丹明B光催化降解,该实验过程如下:
称取获得的氧化铌纳米材料100毫克,黑暗下分散于100毫升浓度为10ppm的罗丹明B溶液中,置于太阳光照射下(波长范围320nm~780nm),每隔一定时间取样、离心后测定上清液残余罗丹明B浓度,获得可见光照射下,该材料的光催化降解曲线。
实施例3
将实施例1和对比例1所得氧化铌纳米材料用于二氧化碳的光催化转化,该实验过程如下:
称取获得的氧化铌纳米材料100毫克,黑暗下分散于装有100毫升去离子水的反应器中,向反应器中持续通入二氧化碳后置于太阳光照射下(波长范围320nm~780nm),经进样器进样及气象色谱仪分析后,获得太阳光照射下,该材料的二氧化碳转化性能。
图1为实施例1的多孔氧化铌纳米材料X射线衍射图谱。由图1可以看出,本发明得到的多孔氧化铌纳米光催化剂材料以六方相氧化铌的形式存在。
图2所示为实施例1的多孔氧化铌纳米材料的透射电镜照片图。由图2可以看出,本发明方法制备的得到的多孔氧化铌纳米光催化剂材料平均粒径小同时有着多孔的微观形貌。
图3所示为实施例1和对比例1中所获得的氧化铌材料对于水溶液中罗丹明B的降解曲线。由图3可以看出,实施例1制备的多孔氧化铌纳米材料在可见光照射下,表现出比对比例1简单沉淀法获得的氧化铌更为优异的光催化降解性能,水溶液中的罗丹明B浓度随着处理时间的延长而减小,120分钟内就能使溶液近90%的罗丹明B被降解,此时罗丹明B的残余浓度仅为初始浓度的11%。
图4为实施例1和对比例1中氧化铌纳米材料对于二氧化碳的光催化转化性能。由图4可以看出,实施例1制备的多孔氧化铌纳米材料在光照条件下,表现出明显的二氧化碳光催化转化性能,可将溶液中的二氧化碳转化为乙烯。
实施例结果表明,本发明利用驱体配制—模板热解—洗涤干燥的工艺流程,成功获得晶粒尺寸细小、具有多孔微观结构的氧化铌纳米材料,从而氧化铌光催化材料的光催化性能,该氧化铌纳米材料在太阳光照射下,具有优异的光催化降解性能和光催化二氧化碳转化性能。上述实例仅作参考,具有和本发明相似或者从本专利思路出发而延伸的提高氧化物材料比表面积和微观孔结构的方法,均在本发明的保护范围。
Claims (7)
1.一种多孔氧化铌纳米材料,其特征在于:所述多孔氧化铌纳米材料为六方晶体结构,晶粒尺寸为5-50nm,具有纳米孔的微观结构。
2.按照权利要求1所述的多孔氧化铌纳米材料的制备方法,其特征在于:该多孔氧化铌纳米材料是通过前驱体配制—模板热解—洗涤干燥的工艺流程制备获得的。
3.按照权利要求2所述的多孔氧化铌纳米材料的制备方法,具体包括步骤:
(1)前驱体配制:首先配置1-1000mmol/L的铌盐溶液,随之将其缓慢滴入碳酸铵固体粉末中,获得模板热解的混合体系;
(2)模板热解:将步骤(1)获得的混合体系置于300~600℃温度下保温0.5-20h;
(3)洗涤干燥:将经步骤(2)模板热解后所得粉末用二次去离子水和无水乙醇交替洗涤5~8次,放入干燥箱在40~120℃温度下干燥一天,即得到所述多孔氧化铌纳米材料。
4.按照权利要求3所述的多孔氧化铌纳米材料的制备方法,其特征在于:步骤(1)中用于配制铌盐溶液的溶剂为水、酒精和乙二醇中的一种或几种,铌盐为氯化铌或乙酸铌。
5.按照权利要求3所述的多孔氧化铌纳米材料的制备方法,其特征在于:步骤(1)中,所述铌盐溶液中的铌盐与碳酸铵固体粉末的重量比例为1:(10-50)。
6.按照权利要求1所述的多孔氧化铌纳米材料在碳中和中的应用,其特征在于:将所述多孔氧化铌纳米材料直接应用于有机染料的光催化降解。
7.按照权利要求1所述的多孔氧化铌纳米材料在碳中和中的应用,其特征在于:将所述多孔氧化铌纳米材料直接应用于二氧化碳的光催化转化,可将二氧化碳转化为烯烃。
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