CN112517046A - 一种基于双致孔剂合成的多级孔氮掺杂碳氧还原催化剂的普适性制备方法 - Google Patents
一种基于双致孔剂合成的多级孔氮掺杂碳氧还原催化剂的普适性制备方法 Download PDFInfo
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Abstract
本发明公开了一种基于双致孔剂合成的多级孔氮掺杂碳氧还原催化剂的普适性制备方法,将生物质蒲苇、柠檬酸锌和氢氧化钾充分研磨得到均匀混合的物料A;将物料A转移至瓷舟中并将瓷舟平放于管式炉内,在惰性气体保护下,由室温经过55min升温至300℃并保持60min,再以5℃/min的升温速率升温至850℃并保持120min,自然降温至室温得到物料B;将物料B转移至烧杯内并倒入盐酸溶液浸泡12h,再用高纯水洗涤至呈中性,然后置于鼓风干燥箱内于60℃干燥12h得到多级孔氮掺杂碳氧还原催化剂。本发明引入氢氧化钾和柠檬酸锌为双致孔剂,能够在碳材料表面制造形成微孔以及不同尺寸范围的介孔,暴露更多的活性位点,增强碳材料的催化,有利于电化学降解活性性能的提高。
Description
技术领域
本发明属于多级孔碳材料的合成技术领域,具体涉及一种基于双致孔剂合成的多级孔氮掺杂碳氧还原催化剂的普适性制备方法。
背景技术
在纺织、印刷和化妆品等行业中,染料是被广泛使用的环境污染物之一,随着染料使用量的增加,高浓度染料废水的排放已经造成严重的环境污染。由于大部分有害染料污染物成分复杂、种类繁多、结构稳定,用一般的处理方法难以得到较好的效果,因此大幅度地增加了有机废水的降解难度。
目前应用于处理环境染料废水的方法主要包括生物法、物理法和化学法等。然而这些方法很多对于有毒性、难降解的污染物处理效果不明显,这些有毒的染料污染物在氧化、羟基化或是其它化学反应作用下,还会形成一些副产物,对环境和人类的健康造成威胁。近年来,高级氧化法因其具有简单、高效、快速等优点而备受关注。其中,针对传统芬顿法中H2O2运输困难、成本高等问题,电芬顿法因能直接原位产生芬顿试剂用于氧化降解有机污染物而备受关注。电芬顿降解体系中,阴极材料的特性起着至关重要的作用。具有高比表面积的多孔碳材料作为阴极广泛地应用于降解有机污染物体系。制备多孔碳材料方式中,氢氧化钾作为常见的致孔剂,易产生微孔和小介孔结构,同时使材料具备高的比表面积。此外,柠檬酸锌可自分解为H2O、COx等小分子气体,同时锌物种在高温下可分解为Zn(OH)2、ZnO、Zn单质等,通过酸洗能够实现造孔作用,产生微孔和相对较大的介孔结构。基于此,本发明将氢氧化钾和柠檬酸锌两种致孔剂结合使用,以期能够制备出比表面积较高、孔径分布范围广且染料降解性能较好的碳材料。
发明内容
本发明解决的技术问题是提供了一种简单高效、绿色清洁且成本低廉的基于双致孔剂合成的多级孔氮掺杂碳氧还原催化剂的普适性制备方法。
本发明为解决上述技术问题采用如下技术方案,一种基于双致孔剂合成的多级孔氮掺杂碳氧还原催化剂的普适性制备方法,其特征在于具体步骤为:
步骤S1:将生物质蒲苇、柠檬酸锌和氢氧化钾按质量比1:5:3在玻璃研钵中充分研磨10min得到均匀混合的物料A;
步骤S2:将步骤S1得到的物料A转移至瓷舟中并将瓷舟平放于管式炉内,在惰性气体保护下,由室温经过55min升温至300℃并保持60min,再以5℃/min的升温速率升温至850℃并保持120min,然后自然降温至室温得到物料B;
步骤S3:将步骤S2得到的物料B转移至烧杯内并倒入盐酸溶液浸泡12h,再用高纯水洗涤至呈中性,然后置于鼓风干燥箱内于60℃干燥12h得到多级孔氮掺杂碳氧还原催化剂,该多级孔氮掺杂碳氧还原催化剂比表面积达到2991m2/g,孔径分布为4.2nm、11.6nm、16.0nm、26.9nm。
进一步限定,步骤S2中所述惰性气体为氮气。
进一步限定,步骤S3中所述盐酸溶液的浓度为2mol/L。
本发明与现有技术相比具有以下有益效果:1、生物质仅与氢氧化钾混合时,比表面积为2628m2/g,孔径分布主要集中在3.1nm、3.9nm。生物质仅与柠檬酸锌混合作用时,比表面积为1186m2/g,孔径分布主要集中在7.7nm。生物质与双致孔剂(柠檬酸锌和氢氧化钾)作用时,由于两种造孔剂造孔位点相同、造孔位点相近造成位点坍塌等原因,相较于单一致孔剂而言,比表面积增加到2991m2/g,孔径分布扩大到4.2nm、11.6nm、16.0nm、26.9nm,将其作为阴极催化剂应用到电芬顿体系中相比较而言具有最高的降解效率,且在使用的过程中不会造成二次污染,对环境友好。2、本发明引入氢氧化钾和柠檬酸锌为双致孔剂,能够在碳材料表面制造形成微孔以及不同尺寸范围的介孔,暴露更多的活性位点,增强碳材料的催化,有利于电化学降解活性性能的提高。
附图说明
图1是实施例1-3制备的目标产物C1-C3吸脱附曲线图和孔径分布图;
图2是实施例3-5制备的目标产物C3-C5的X射线衍射图谱;
图3是实施例3-5制备目标产物C3-C5的Raman图谱;
图4是实施例3-5制备的目标产物C3-C5的X射线光电子全谱图;
图5是实施例1-3制备的目标产物C1-C3的不同材料的降解时间图。
具体实施方式
以下通过实施例对本发明的上述内容做进一步详细说明,但不应该将此理解为本发明上述主题的范围仅限于以下的实施例,凡基于本发明上述内容实现的技术均属于本发明的范围。
实施例1
步骤S1:将1g生物质蒲苇与5g柠檬酸锌充分混合均匀后得到物料A1;
步骤S2:将步骤S1得到的物料A1转移至瓷舟中并将瓷舟平放于管式炉内,在惰性气体保护下,由室温经过55min升温至300℃并保持60min,再以5℃/min的升温速率升温至850℃并保持120min,然后自然降温至室温得到物料B1;
步骤S3:将步骤S2得到的物料B1转移至烧杯内并倒入盐酸溶液浸泡12h,再用高纯水洗涤呈中性,然后置于鼓风干燥箱内于60oC干燥12h得到目标产物C1;
步骤S4:将制得的双致孔剂合成的多孔氮掺杂碳催化剂C1用作电芬顿体系的阴极催化剂去降解50mL浓度为15mg/L罗丹明B溶液,降解彻底所用时间为8100s。
实施例2
步骤S1:将1g生物质蒲苇与3g氢氧化钾充分混合均匀后得到物料A2;
步骤S2:将步骤S1得到的物料A2转移至瓷舟中并将瓷舟平放于管式炉内,在惰性气体保护下,由室温经过55min升温至300℃并保持60min,再以5℃/min的升温速率升温至850℃并保持120min,然后自然降温至室温得到物料B2;
步骤S3:将步骤S2得到的物料B2转移至烧杯内并倒入盐酸溶液浸泡12h,再用高纯水洗涤呈中性,然后置于鼓风干燥箱内于60oC干燥12h得到目标产物C2;
步骤S4:将制得的双致孔剂合成的多孔氮掺杂碳催化剂C2用作电芬顿体系的阴极催化剂去降解50mL浓度为15mg/L罗丹明B溶液,降解彻底所用时间为7200s。
实施例3
步骤S1:将1g生物质蒲苇、3g氢氧化钾和5g柠檬酸锌充分混合均匀后得到物料A3;
步骤S2:将步骤S1得到的物料A3转移至瓷舟中并将瓷舟平放于管式炉内,在惰性气体保护下,由室温经过55min升温至300℃并保持60min,再以5℃/min的升温速率升温至850℃并保持120min,然后自然降温至室温得到物料B3;
步骤S3:将步骤S2得到的物料B3转移至烧杯内并倒入盐酸溶液浸泡12h,再用高纯水洗涤呈中性,然后置于鼓风干燥箱内于60oC干燥12h得到目标产物C3;
步骤S4:将制得的双致孔剂合成的多孔氮掺杂碳催化剂C3用作电芬顿体系的阴极催化剂去降解50mL浓度为15mg/L罗丹明B溶液,降解彻底所用时间为2000s。
实施例4
步骤S1:将1g生物质蒲苇、3g氢氧化钾和5g柠檬酸锌充分混合均匀后得到物料A4;
步骤S2:将步骤S1得到的物料A4转移至瓷舟中并将瓷舟平放于管式炉内,在惰性气体保护下,由室温经过55min升温至300℃并保持60min,再以5℃/min的升温速率升温至850℃并保持120min,然后自然降温至室温得到物料B4;
步骤S3:将步骤S2得到的物料B4转移至烧杯内并倒入盐酸溶液浸泡12h,再用高纯水洗涤呈中性,然后置于鼓风干燥箱内于60℃干燥12h得到目标产物C4;
步骤S4:将制得的双致孔剂合成的多孔氮掺杂碳催化剂C4用作电芬顿体系的阴极催化剂去降解50mL浓度为15mg/L铬蓝黑R,降解彻底所用时间为1000s。
实施例5
步骤S1:将1g生物质蒲苇、3g氢氧化钾和5g柠檬酸锌充分混合均匀后得到物料A5;
步骤S2:将步骤S1得到的物料A5转移至瓷舟中并将瓷舟平放于管式炉内,在惰性气体保护下,由室温经过55min升温至300℃并保持60min,再以5℃/min的升温速率升温至850℃并保持120min,然后自然降温至室温得到物料B5;
步骤S3:将步骤S2得到的物料B5转移至烧杯内并倒入盐酸溶液浸泡12h,再用高纯水洗涤呈中性,然后置于鼓风干燥箱内于60℃干燥12h得到目标产物C5;
步骤S4:将制得的双致孔剂合成的多孔氮掺杂碳催化剂C5用作电芬顿体系的阴极催化剂去降解50mL浓度为15mg/L罗丹明B溶液和铬蓝黑R的混合染料,降解彻底所用时间为2100s。
以上显示和描述了本发明的基本原理,主要特征和优点,在不脱离本发明精神和范围的前提下,本发明还有各种变化和改进,这些变化和改进都落入要求保护的本发明的范围。
Claims (3)
1.一种基于双致孔剂合成的多级孔氮掺杂碳氧还原催化剂的普适性制备方法,其特征在于具体步骤为:
步骤S1:将生物质蒲苇、柠檬酸锌和氢氧化钾按质量比1:5:3在玻璃研钵中充分研磨10min得到均匀混合的物料A;
步骤S2:将步骤S1得到的物料A转移至瓷舟中并将瓷舟平放于管式炉内,在惰性气体保护下,由室温经过55min升温至300℃并保持60min,再以5℃/min的升温速率升温至850℃并保持120min,然后自然降温至室温得到物料B;
步骤S3:将步骤S2得到的物料B转移至烧杯内并倒入盐酸溶液浸泡12h,再用高纯水洗涤至呈中性,然后置于鼓风干燥箱内于60℃干燥12h得到多级孔氮掺杂碳氧还原催化剂,该多级孔氮掺杂碳氧还原催化剂比表面积达到2991m2/g,孔径分布为4.2nm、11.6nm、16.0nm、26.9nm。
2.根据权利要求1所述的基于双致孔剂合成的多级孔氮掺杂碳氧还原催化剂的普适性制备方法,其特征在于:步骤S2中所述惰性气体为氮气。
3.根据权利要求1所述的基于双致孔剂合成的多级孔氮掺杂碳氧还原催化剂的普适性制备方法,其特征在于:步骤S3中所述盐酸溶液的浓度为2mol/L。
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