CN114196984A - 一种碳纸上恒电流电沉积铜基催化剂及其制备方法和在电催化4-乙炔基苯胺中的应用 - Google Patents
一种碳纸上恒电流电沉积铜基催化剂及其制备方法和在电催化4-乙炔基苯胺中的应用 Download PDFInfo
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Abstract
本发明涉及催化剂技术领域,具体涉及一种碳纸上恒电流电沉积铜基催化剂及其制备方法和在电催化4‑乙炔基苯胺中的应用。制备方法包括如下步骤,泡沫铜清洗后干燥,将碳纸用硝酸浸泡后清洗干净,干燥后进行煅烧;将H2SO4与CuSO4混合得混合液;以泡沫铜作为对电极,碳纸作为工作电极,混合液作为电解液,通过恒电流沉积,在碳纸电沉积得到铜基催化剂。所述的铜基催化剂以水作为氢源,利用电解水产生的氢还原炔烃,既可以有效利用不易储存运输的氢,又能避免使用H2或者有毒氢源。使用廉价金属催化剂催化炔烃半氢化可以降低成本,实现高的经济效益。
Description
技术领域
本发明涉及催化剂技术领域,具体涉及一种碳纸上恒电流电沉积铜基催化剂及其制备方法和在电催化4-乙炔基苯胺中的应用。
背景技术
选择性加氢是精细化学品、药品、食品和农用化学品工业生产的核心。炔烃的选择性半氢化能够生产具有高附加值的烯烃产物,在化工生产中是非常重要的。传统的半氢化反应已经取得了重大进展,但目前对电催化炔烃半氢化的报告较少,而且其主要依赖于昂贵的贵金属催化剂,使用H2或者昂贵有毒的有机氢源,在成本,安全和环境方面存在严重问题。
发明内容
本发明通过恒电流电化学沉积在碳纸上制备了一种铜基催化剂,以水为氢源,在碱性电解液中电催化炔烃制备烯烃,烯烃能达到95%的选择性。
为实现上述目的,本发明的技术方案如下:一种碳纸上恒电流电沉积铜基催化剂,制备方法包括如下步骤,
1)将泡沫铜清洗后干燥,将碳纸用硝酸浸泡后清洗干净,干燥后进行煅烧;
2)将H2SO4与CuSO4混合得混合液;
3)以泡沫铜作为对电极,碳纸作为工作电极,混合液作为电解液,通过恒电流沉积,在碳纸电沉积得到铜基催化剂。
上述的一种碳纸上恒电流电沉积铜基催化剂,步骤1)中,煅烧温度为400℃,煅烧时间为5h。
上述的一种碳纸上恒电流电沉积铜基催化剂,步骤2)中,按摩尔比,H2SO4:CuSO4=6:1。
上述的一种碳纸上恒电流电沉积铜基催化剂,步骤3)中,沉积条件为-0.05A,沉积时间为80s。
上述的一种碳纸上恒电流电沉积铜基催化剂以水为氢源电催化炔烃半氢化制备烯烃。
上述的应用,方法如下:采用H型电解池,在阴极电解池中进行电催化反应,电解的底物为4-乙炔基苯胺,加入共溶剂,进行电化学实验,电催化4-乙炔基苯胺生成4-乙烯基苯胺,电化学实验中参比电极为Ag/AgCl电极,对电极为铂电极,上述的碳纸上恒电流电沉积铜基催化剂为工作电极。
上述的应用,所述H型电解池中,阴极电解池电解液为:KOH溶液,阳极电解池电解液为KOH溶液,阴极和阳极电解池之间通过质子交换膜连接。
上述的应用,所述的共溶剂为1,4-二氧六环。
本发明的有益效果:本发明以水作为氢源,利用电解水产生的氢还原炔烃,既可以有效利用不易储存运输的氢,又能避免使用H2或者有毒氢源。使用廉价金属催化剂催化炔烃半氢化可以降低成本,实现高的经济效益。
附图说明
图1为电沉积铜基催化剂的扫描电镜图。
图2为电沉积铜基催化剂的X射线衍射图(XRD)。
图3为电沉积铜基催化剂和碳纸电催化炔烃半氢化的线性扫描伏安曲线。
具体实施方式
实施例1
制备铜基催化剂:首先对买来的商用泡沫铜进行预处理:依次用3M盐酸,丙酮,乙醇,水,各洗涤10min,然后在60℃烘箱中干燥;碳纸的预处理:碳纸切割成1×2cm,用硝酸浸泡30min,用去离子水冲洗干净,吹干,在马弗炉中400℃烧5h;2M H2SO4 12mL,0.2M CuSO4,20mL,混合;取10mL混合后的溶液作为电解液,预处理之后的泡沫铜,作为对电极;碳纸作为工作电极,通过恒电流电沉积在碳纸上制备铜基催化剂,沉积条件为-0.05A,80s,将沉积后的碳纸在去离子水中浸泡30min,除去无机盐,然后在室温下干燥,得到铜基催化剂。电化学工作站型号为CHI 760E,参比电极为Ag/AgCl电极,线性扫描伏安扫描参数为旋转速率1600rpm、扫描速率为10mV s-1。从图1中可以看出催化剂为不规则颗粒。从图2中的XRD 图可以看出,17.98处的峰对应为Cu4O3;43.47,50.41,74.13处的峰对应为金属Cu,说明成功沉积了铜基催化剂,沉积的铜基催化剂中铜为0价,+1价,+2价的变价。
电极的电化学性能测试:采用CHI760电化学工作站测试电化学沉积的铜基催化剂的电化学性能。采用H型电解池和三电极工作系统进行了电化学性能测试。以1M KOH为电解液,阳极室和阴极室分别加入15mL电解液,并且在阴极室加入2.4mg的4-乙炔基苯胺和1.07ml的1,4-二氧六环。电沉积的催化剂电极为工作电极,碳棒为对电极,Ag/AgCl电极为参比电极。将电解池密封,向液面中通入氮气30min,以除去溶液中的氧气,选择LSV测试,进行电化学性能测试。电沉积的铜基催化剂在-0.56V vs.RHE时,电流密度可达到29mA/cm2,碳纸在-0.56V vs.RHE时,电流密度仅为2.8mA/cm2,在-0.56V vs.RHE时,所制备的铜基催化剂的电流密度约为碳纸的10倍。本文中所用的电压以标准氢电极电势为基准。
电沉积的碳纸用去离子水清洗后,在室温下干燥,电化学工作站型号为CHI 760E,选择 IT测试,参比电极为Ag/AgCl电极,对电极为铂电极,线性扫描伏安扫描参数为旋转速率 1600rpm、扫描速率为10mV s-1。
通过对比可以发现,电沉积铜基催化剂的电流密度明显高于碳纸,电沉积铜基催化剂对炔烃半氢化有很好的催化效果。
实施例2
以水为氢源,电催化炔烃半氢化制备烯烃。采用H型电解池,在阴极电解池中,电解液为:13.93ml 1M KOH;阳极电解池电解液为15ml1M KOH溶液。阴极和阳极电解池之间通过质子交换膜连接。在阴极电解池中进行电催化反应,电解的底物为2.4mg4-乙炔基苯胺,加入共溶剂1.07ml 1,4-二氧六环后溶于KOH溶液中,进行电化学实验,电催化4-乙炔基苯胺生成4-乙烯基苯胺。电化学工作站型号为CHI 760E,参比电极为Ag/AgCl电极,对电极为碳棒,沉积的铜基催化剂为工作电极,线性扫描伏安扫描参数为旋转速率1600rpm、扫描速率为10mV s-1。图1的LSV曲线显示,-0.56V vs.RHE电压下,沉积的铜基催化剂的电流密度最大。在碱性环境中,通过计时电流法电催化炔烃选择性生成烯烃,在-0.56V vs.RHE电压下,电解5h,转速300r/min。电解后的电解液,用二氯甲烷萃取,进气相,通过内标法,检测烯烃产物的选择性可达95%。
Claims (8)
1.一种碳纸上恒电流电沉积铜基催化剂,其特征在于,制备方法包括如下步骤,
1)将泡沫铜清洗后干燥;将碳纸用硝酸浸泡后清洗干净,干燥后进行煅烧;
2)将H2SO4与CuSO4混合得混合液;
3)以泡沫铜作为对电极,碳纸作为工作电极,混合液作为电解液,通过恒电流沉积,在碳纸电沉积得到铜基催化剂。
2.根据权利要求1所述的一种碳纸上恒电流电沉积铜基催化剂,其特征在于,步骤1)中,煅烧温度为400℃,煅烧时间为5h。
3.根据权利要求1所述的一种碳纸上恒电流电沉积铜基催化剂,其特征在于,步骤2)中,按摩尔比,H2SO4:CuSO4=6:1。
4.根据权利要求1所述的一种碳纸上恒电流电沉积铜基催化剂,其特征在于,步骤3)中,沉积条件为-0.05A,沉积时间为80s。
5.权利要求1所述的一种碳纸上恒电流电沉积铜基催化剂以水为氢源电催化炔烃半氢化制备烯烃。
6.根据权利要求5所述的应用,其特征在于,方法如下:采用H型电解池,在阴极电解池中进行电催化反应,电解的底物为4-乙炔基苯胺,加入共溶剂,进行电化学实验,电催化4-乙炔基苯胺生成4-乙烯基苯胺,电化学实验中参比电极为Ag/AgCl电极,对电极为铂电极,权利要求1所述的碳纸上恒电流电沉积铜基催化剂为工作电极。
7.根据权利要求6所述的应用,其特征在于,所述H型电解池中,阴极电解池电解液为:KOH溶液,阳极电解池电解液为KOH溶液,阴极和阳极电解池之间通过质子交换膜连接。
8.根据权利要求7所述的应用,其特征在于,所述的共溶剂为1,4-二氧六环。
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