CN114134530A - Cu-P-100催化剂的制备方法及其在二氧化碳电催化还原中的应用 - Google Patents
Cu-P-100催化剂的制备方法及其在二氧化碳电催化还原中的应用 Download PDFInfo
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Abstract
本发明涉及Cu‑P‑100催化剂的制备方法及其在二氧化碳电催化还原中的应用。制备方法包括如下步骤:首先将碳纸浸入盐酸中,超声洗涤后取出碳纸,依次用去离子水、丙酮、去离子水超声洗涤,烘干,将烘干后的碳纸裁剪成1cm×2cm的长方形,即得到处理好的碳纸;其次将单宁酸和硝酸完全溶解于离子水中得到电沉积液;最后利用电化学工作站向处理好的碳纸施加5mA的恒电流,沉积180s,取出沉积后的碳纸,用乙醇冲洗,用氮气吹干,得到Cu‑P‑100催化剂。本发明制备的Cu‑P‑100催化剂能将二氧化碳还原成乙酸,乙酸的法拉第效率较高。
Description
技术领域
本发明属于催化材料技术领域,具体涉及Cu-P-100催化剂的制备方法及其在二氧化碳电催化还原中的应用。
背景技术
二氧化碳的电催化还原反应(CO2RR)不仅可以减轻温室效应,还可以生产出具有较高价值化合物充当燃料来缓解化石能量危机。然而,二氧化碳分子非常稳定,想将二氧化碳分子还原成其他碳产物需要很高的能量。迄今为止,将二氧化碳分子还原成如一氧化碳、甲酸等转移两个电子的各种催化剂的法拉第效率已经可以达到95%以上。但进一步将二氧化碳转化为碳原子数在两个以上的具有更高商业价值的产品,包括乙烯、乙醇、乙酸、丙醇等,催化剂的活性和选择性仍是一个巨大的挑战。一氧化碳是二氧化碳还原过程中最重要的中间体,而Cu因其与CO的结合被认为是电化学催化CO2生成C2+产物的唯一金属。因此,人们开发了各种方法和策略来设计制备铜基催化剂。其中,电沉积作为一种清洁、简单的操作技术,在添加剂的辅助下制备出性能良好的铜基催化剂。
发明内容
为解决上述问题,本发明采用的技术方案为:Cu-P-100催化剂的制备方法,包括如下步骤:
1)将碳纸置于烧杯中,加入盐酸,使盐酸没过碳纸,超声洗涤10min后取出碳纸,用去离子水超声洗涤10min两次,用丙酮超声洗涤10min,再用去离子水超声洗涤10min两次,取出碳纸置于真空干燥箱中烘干,将烘干后的碳纸裁剪成1cm×2cm的长方形,即得到处理好的碳纸;
2)将单宁酸和硝酸铜置于烧杯中,加入20mL去离子水,超声搅拌使其完全溶解,即得到电沉积液;
3)在装有电沉积液的烧杯中加入磁子以恒定转速保持搅拌,防止电沉积液分层,以Ag/AgCl为参比电极、以石墨棒为对电极,将步骤1)得到的处理好的碳纸夹在电极夹上作为工作电极,利用电化学工作站向夹在电极夹上的碳纸施加的恒电流,沉积180s,取出沉积后的碳纸,用乙醇冲洗,用氮气吹干,得到Cu-P-100催化剂。
进一步的,上述的制备方法,步骤1)中,所述盐酸的浓度为0.1mol/L。
进一步的,上述的制备方法,步骤2)中,所述单宁酸的质量为0.17g。
进一步的,上述的制备方法,步骤2)中,所述硝酸铜的质量为0.48g。
进一步的,上述的制备方法,步骤3)中,所述利用电化学工作站向夹在电极夹上的碳纸施加的恒电流为5mA。
本发明提供的制备方法制备的Cu-P-100催化剂在二氧化碳电催化还原中的应用。
本发明的有益效果为:
1、本发明制备的Cu-P-100催化剂能将二氧化碳还原成乙酸,乙酸的法拉第效率较高,可达到33.4%。
2、本发明制备方法操作简单,并且清洁环保。
3、本发明制备的Cu-P-100催化剂在-0.9V vs.RHE的电位下其总法拉第效率最高,可达近65%。
附图说明
图1为Cu-P-100催化剂的扫描电镜图。
图2为Cu-P-100催化剂的X射线衍射(XRD)谱图。
图3为Cu-P-100催化剂在二氧化碳和氩气条件下的线性扫描伏安特性曲线图。
图4为Cu-P-100催化剂电催化还原二氧化碳产物的法拉第效率图。
具体实施方式
实施例1 Cu-P-100催化剂的制备
1)将碳纸置于烧杯中,加入0.1mol/L盐酸,使盐酸没过碳纸,超声洗涤10min后取出碳纸,用去离子水超声洗涤10min两次,用丙酮超声洗涤10min,再用去离子水超声洗涤10min两次,取出碳纸置于真空干燥箱中烘干,将烘干后的碳纸裁剪成1cm×2cm的长方形,即得到处理好的碳纸;
2)将0.17g单宁酸和0.48g硝酸铜置于烧杯中,加入20mL去离子水,超声搅拌使其完全溶解,即得到电沉积液;
3)在装有电沉积液的烧杯中加入磁子以恒定转速保持搅拌,防止电沉积液分层,以Ag/AgCl为参比电极、以石墨棒为对电极,将步骤1)得到的处理好的碳纸夹在电极夹上作为工作电极,利用电化学工作站向夹在电极夹上的碳纸施加5mA的恒电流,沉积180s,取出沉积后的碳纸,用乙醇冲洗,用氮气吹干,得到Cu-P-100催化剂。
4)电化学性能测试
利用电化学工作站CHI760E,采用三电极体系进行电化学性能测试,其中以铂丝作为对电极,Ag/AgCl(饱和KCl)作为参比电极,负载催化剂的碳纸夹在电极夹上作为工作电极,电解池选用典型的H型电解池,将用超纯水洗过的质子交换膜(Nafion 177)放入电解池两隔室中间以确保仅使氢离子得以通过,每个隔室中电解液的液面需保持水平,均配制0.1mol/L的KHCO3的溶液作为电解液,溶剂必须为超纯水要尽量排除氯离子、硝酸根离子、硫酸根离子等杂离子干扰。所有测试均在室温条件下用转子流量计控制通入30min流量为25sccm的高纯度氩气,然后再通入相同流量和时间的高纯度二氧化碳。根据能斯特方程,在所有参比与Ag/AgCl电极测得的所有电势均需转化为相对于可逆氢电极(RHE)的电势:ERHE=EAg/AgCl+0.059×pH+0.197V。
5)电催化还原二氧化碳性能测试
利用制备好的Cu-P-100催化剂进行电催化还原二氧化碳,将测试用的H形电解池在稀盐酸中浸泡10min,目的是为了除去电解池中其他物质,组装好H形电解池后,在电解池的两隔室中加入50mL用超纯水配制的0.1mol/L的KHCO3溶液,密封好,在阴极室通入30min流量25sccm的高纯度氩气,然后再通入与前面相同流量和时间的高纯度二氧化碳,在不同电位下进行电解反应,在此期间控制二氧化碳的流量稳定在25sccm不变,每20min收集一次反应产生的气体,每个电位收集三次共1h,记录反应时施加的总电荷量,将收集到的气体通入气质联用仪,测出其气态产物量和种类。
图1为Cu-P-100催化剂的扫描电镜图,从图1中可以看到整个碳纸基材都被团聚的颗粒所覆盖,图中展示了每一个团聚颗粒的表面都是由很多立方体纳米颗粒所构成。
图2为Cu-P-100催化剂的X射线衍射(XRD)谱图。
图3为Cu-P-100催化剂在二氧化碳和氩气条件下的线性扫描伏安特性曲线(LSV),通过对比可以发现,在二氧化碳条件下的电流密度更高,表明其对二氧化碳有一定的催化还原作用。
图4为Cu-P-100催化剂电催化还原二氧化碳产物的法拉第效率图,从图4中可以看到,在-0.9V vs.RHE的条件下,乙酸的法拉第效率最高,达到33.4%。
Claims (6)
1.Cu-P-100催化剂的制备方法,其特征在于,制备方法包括如下步骤:
1)将碳纸置于烧杯中,加入盐酸,使盐酸没过碳纸,超声洗涤10min后取出碳纸,用去离子水超声洗涤10min两次,用丙酮超声洗涤10min,再用去离子水超声洗涤10min两次,取出碳纸置于真空干燥箱中烘干,将烘干后的碳纸裁剪成1cm×2cm的长方形,即得到处理好的碳纸;
2)将单宁酸和硝酸铜置于烧杯中,加入20mL去离子水,超声搅拌使其完全溶解,即得到电沉积液;
3)在装有电沉积液的烧杯中加入磁子以恒定转速保持搅拌,防止电沉积液分层,以Ag/AgCl为参比电极、以石墨棒为对电极,将步骤1)得到的处理好的碳纸夹在电极夹上作为工作电极,利用电化学工作站向夹在电极夹上的碳纸施加的恒电流,沉积180s,取出沉积后的碳纸,用乙醇冲洗,用氮气吹干,得到Cu-P-100催化剂。
2.根据权利要求1所述的制备方法,其特征在于,步骤1)中,所述盐酸的浓度为0.1mol/L。
3.根据权利要求1所述的制备方法,其特征在于,步骤2)中,所述单宁酸的质量为0.17g。
4.根据权利要求1所述的制备方法,其特征在于,步骤2)中,所述硝酸铜的质量为0.48g。
5.根据权利要求1所述的制备方法,其特征在于,步骤3)中,所述利用电化学工作站向夹在电极夹上的碳纸施加的恒电流为5mA。
6.根据权利要求1所述的制备方法制备的Cu-P-100催化剂在二氧化碳电催化还原中的应用。
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