CN111204848B - 一种导电基底负载金属的非均匀阴极电还原去除污染物的方法 - Google Patents
一种导电基底负载金属的非均匀阴极电还原去除污染物的方法 Download PDFInfo
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Abstract
本发明提供了一种导电基底负载金属的非均匀阴极电还原去除污染物的方法,步骤如下:非贵金属A和贵金属B在三维导电材料上分段负载,采用真空抽滤或浸渍的方式制备导电基底负载金属的非均匀电极。导电基底材料选择范围广,可以是金属,碳材料,导电膜等材料。导电基底材料上非贵金属A和贵金属B浓度占比逐渐变化,使得不同金属充分发挥其作用,高效去除水中污染物。导电基底材料上非贵金属A和贵金属B的比例可调节,灵活性高。在电化学反应器中,将金属负载平板电极按顺序组合成三维整体非均匀阴极,使污染物首先被吸附还原为中间产物,再被还原为无毒无害的物质,充分发挥非贵金属A和贵金属B的作用,提高污染物去除率及产物选择性。
Description
技术领域
本发明涉及一种导电基底负载金属的非均匀阴极电还原去除污染物的方法。具体是一种金属负载的非均匀三维阴极,或由金属负载的平板电极组成的三维整体非均匀阴极,在直流电的作用下,电还原去除水中污染物,属于环境功能材料及水处理应用技术领域。
背景技术
电还原法是一种高效去除水中污染物的方法,电极通过催化剂的修饰,可以提高污染物的去除率及还原反应的选择性。传统的阴极是在导电材料表面均匀负载催化剂来提高电极的催化活性。而非均匀阴极的设计是使导电基底上催化剂的浓度比例逐渐变化,适用于还原反应分步进行的物质,在反应的不同阶段提供比例不同的催化剂,充分发挥其催化作用,提高去除率及产物选择性。
发明内容
本发明的目的是设计一种三维导电基底负载金属非均匀阴极,或在反应器中按顺序放置金属负载平板电极,组成三维整体非均匀电极,电还原水中的污染物,建立一种高效去除污染物的方法。
本发明的技术方案:
一种导电基底负载金属的非均匀阴极电还原去除污染物的方法,步骤如下:
非贵金属A和贵金属B在三维导电材料上分段负载,采用真空抽滤或浸渍的方式,包括以下步骤:
(1)配置一定比例的含非贵金属A和贵金属B的盐溶液,取清洗好的导电基底材料,将不需负载金属的部分用生料带封住,然后将其真空抽滤或浸渍;
(2)改变生料带封装位置,配置另一比例的含非贵金属A和贵金属B的盐溶液,重复上述操作;
(3)将处理后负载金属离子的导电基底材料置于300~500℃温度条件下煅烧2小时,升温速率5℃/min;
(4)煅烧后放入2 wt %~5wt%硼氢化钠溶液中,还原1~4小时,取出后用超纯水清洗掉多余的NaBH4,烘干,即得导电基底负载金属的非均匀电极,该导电基底负载金属的非均匀电极的一端向另一端中负载的金属由非贵金属A向贵金属B过度,即前段负载非贵金属A的占比最大,中间段负载金属A的占比逐渐较小,贵金属B的占比逐渐增大,后段负载金属B占比最大;
(5)将导电基底负载金属的非均匀电极作为阴极,以IrO2/Ti为阳极,50mg/L的硝酸盐溶液从阳极流向阴极,以流动态的方式降解硝酸盐;在电化学反应器中,硝酸盐溶液先接触非贵金属A含量高的阴极,此时NO3 -在非贵金属表面还原成NO2 -,接着流过贵金属B含量高的阴极,此时NO2 -在贵金属表面进一步还原为N2;电催化降解硝酸盐的电流为80mA,硝酸盐溶液的起始pH为中性,电解质为0.05M Na2SO4溶液。
所述的非贵金属A为Cu、Sn、Zn或Ni。
所述的贵金属B为Pd、Au或Pt。
所述的导电基底材料是金属、碳材料或导电膜。
本发明的有益效果:
(1)导电基底材料选择范围广,可以是金属,碳材料,导电膜等材料。
(2)导电基底材料上金属A和B浓度占比逐渐变化,使得不同金属充分发挥其作用,高效去除水中污染物。
(3)导电基底材料上非贵金属A和贵金属B的比例可调节,灵活性高。
(4)在电化学反应器中,将金属负载平板电极按顺序组合成三维整体非均匀阴极,使污染物首先被吸附还原为中间产物,再被还原为无毒无害的物质,充分发挥非贵金属A和贵金属B的作用,提高污染物去除率及产物选择性。
附图说明
图1是未负载金属的碳纤维毡负载金属的电镜图。
图2是负载金属的碳纤维毡负载金属的电镜图。
图3是木炭负载金属的电镜图。
具体实施方式
以下结合技术方案和附图,进一步说明本发明的具体实施方式。
木炭负载金属钯铜非均匀阴极的制备:炭化松木直径6cm,厚度1cm,首先将木炭三等分,右侧二等份用生料带将封住,露出左侧1/3,然后置于抽滤装置中,配制Pd:Cu=2:1的盐溶液,开始进行抽滤;同样左右两侧用生料带封住,露出中间1/3部分,配制Pd:Cu=4:1的盐溶液,开始进行抽滤;最后左侧2/3部分用生料带封住,露出右侧1/3部分,配制Pd:Cu=6:1的盐溶液,开始进行抽滤。将抽滤好的木炭放入马弗炉内,300℃煅烧2小时,升温速率5℃/min。取出后冷却至室温。称取1.6g硼氢化钠配制成5%的水溶液,放入煅烧后的木炭,还原4小时。取出后用超纯水冲洗,110℃烘干2小时,得到Pd-Cu负载的非均匀阴极,对该电极进行SEM表征,如图3所示。
采用此电极作为阴极进行电还原硝酸盐实验,阳极为IrO2/Ti。硝酸盐溶液体积50mL,初始浓度为25mg/L,电流为80mA,初始pH为中性,添加0.05mol/LNa2SO4电解质,最终出水中硝酸盐氮浓度为1.92mg/L,去除率达到92.32%,亚硝酸盐氮浓度为1.83mg/L,氨氮浓度为15.84mg/L。
实施例2
电极制备与利用此电极降解硝酸盐的方法如实施例1,不同的是,首先将左侧1/3部分露出,将8mmol/L的硝酸铜溶液倒入抽滤装置中,此时Pd:Cu=0:1,然后将中间1/3部分露出,将8mmol/L的硝酸铜和相同体积的硝酸钯(16mmol/L)溶液倒入抽滤装置中,此时Pd:Cu=2:1,最后将右侧1/3部分露出,将16mmol/L硝酸钯溶液倒入抽滤装置中,此时Pd:Cu=1:0。以此电极作为阴极电还原水中硝酸盐,硝酸盐溶液体积50mL,初始浓度为50mg/L,电流为80mA,初始pH为中性,添加0.05mol/LNa2SO4电解质,最终出水中硝酸盐氮浓度为2.33mg/L,去除率达到95.34%,亚硝酸盐氮浓度为0.24mg/L,氨氮浓度为26.05mg/L。
实施例3
电极制备与利用此电极降解硝酸盐的方法如实施例1,不同的是首先将木炭1/2部分浸入到8mmol/L的硝酸铜溶液,再将1/2部分浸入到相同体积的硝酸钯(32mmol/L)溶液中,此时的Pd:Cu=4:1。以此电极作为阴极电还原水中硝酸盐,硝酸盐溶液体积50mL,初始浓度为25mg/L,电流为80mA,初始pH为中性,添加0.05mol/LNa2SO4电解质,最终出水中硝酸盐氮浓度为6.93mg/L,去除率达到72.28%,亚硝酸盐氮浓度为0.72mg/L,氨氮浓度为8.32mg/L。
实施例4
电极制备方法如实施例1,不同的是导电基底材料为碳纤维毡,制备单金属铜负载的电极,将碳纤维毡(4*4cm)浸入到8mmol/L的硝酸铜溶液中,浸渍10小时,将另一块相同面积的碳纤维毡浸入到16mmol/L的硝酸钯溶液中,浸渍10小时,制备成单金属钯电极。将三块碳纤维毡(4*4cm)分别浸入到Pd:Cu=8:1,4:1,2:1溶液中,浸渍煅烧还原后,制成双金属电极,未负载的碳纤维毡电镜图如图1所示,负载金属后的碳纤维毡电镜图如图2所示。
将单金属铜电极,钯铜比为2:1,4:1,8:1,单金属钯电极按叙述顺序置于电化学反应器中,组成整体阴极。利用此电极电还原硝酸盐的方法如下,硝酸盐溶液泵入反应器后,首先流过单金属铜电极,再一次流过钯铜比为2:1,4:1,8:1的阴极,最后流过单金属钯电极,硝酸盐溶液初始浓度为50mg/L,电流为80mA,初始pH为中性,添加0.05mol/LNa2SO4电解质,最终出水中硝酸盐氮浓度为2.79mg/L,去除率达到94.42%,亚硝酸盐氮浓度为5.57mg/L,氨氮浓度为4.23mg/L。
Claims (5)
1.一种导电基底负载金属的非均匀阴极电还原去除污染物的方法,其特征在于,步骤如下:
非贵金属A和贵金属B在三维导电材料上分段负载,采用真空抽滤或浸渍的方式,包括以下步骤:
(1)配制一定比例的含非贵金属A和贵金属B的盐溶液,取清洗好的导电基底材料,将不需负载金属的部分用生料带封住,然后将其真空抽滤或浸渍;
(2)改变生料带封装位置,配制另一比例的含非贵金属A和贵金属B的盐溶液,重复上述操作;
(3)将处理后负载金属离子的导电基底材料置于300~500℃温度条件下煅烧2小时,升温速率5℃/min;
(4)煅烧后放入2wt%~5wt%硼氢化钠溶液中,还原1~4小时,取出后用超纯水清洗掉多余的NaBH4,烘干,即得导电基底负载金属的非均匀电极,该导电基底负载金属的非均匀电极的一端向另一端中负载的金属由非贵金属A向贵金属B过渡,即前段负载非贵金属A的占比最大,中间段负载金属A的占比逐渐较小,贵金属B的占比逐渐增大,后段负载金属B占比最大;
(5)将导电基底负载金属的非均匀电极作为阴极,以IrO2/Ti为阳极,硝酸盐溶液从阳极流向阴极,以流动态的方式降解硝酸盐;在电化学反应器中,硝酸盐溶液先接触非贵金属A含量高的阴极,此时NO3 -在非贵金属表面还原成NO2 -,接着流过贵金属B含量高的阴极,此时NO2 -在贵金属表面进一步还原为N2。
2.根据权利要求1所述的导电基底负载金属的非均匀阴极电还原去除污染物的方法,其特征在于,所述的非贵金属A为Cu、Sn、Zn或Ni。
3.根据权利要求1或2所述的导电基底负载金属的非均匀阴极电还原去除污染物的方法,其特征在于,所述的贵金属B为Pd、Au或Pt。
4.根据权利要求1或2所述的导电基底负载金属的非均匀阴极电还原去除污染物的方法,其特征在于,所述的导电基底材料是金属、碳材料或导电膜。
5.根据权利要求3所述的导电基底负载金属的非均匀阴极电还原去除污染物的方法,其特征在于,所述的导电基底材料是金属、碳材料或导电膜。
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