CN113979518A - 一种用于电催化氧化氨氮的电极及其制备方法和应用 - Google Patents
一种用于电催化氧化氨氮的电极及其制备方法和应用 Download PDFInfo
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- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 230000003647 oxidation Effects 0.000 title claims abstract description 27
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 27
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- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 claims abstract description 29
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 26
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- 238000003756 stirring Methods 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 3
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 3
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 239000011888 foil Substances 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 238000007711 solidification Methods 0.000 claims description 2
- 230000008023 solidification Effects 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 2
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- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 abstract 1
- 229920000642 polymer Polymers 0.000 abstract 1
- 229910052707 ruthenium Inorganic materials 0.000 abstract 1
- BIXNGBXQRRXPLM-UHFFFAOYSA-K ruthenium(3+);trichloride;hydrate Chemical compound O.Cl[Ru](Cl)Cl BIXNGBXQRRXPLM-UHFFFAOYSA-K 0.000 abstract 1
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Abstract
本发明公开了一种用于电催化氧化氨氮电极及其制备方法和应用,该电极是一种钛箔负载氧化钌电极(RuO2/Ti),所述电极包括基底和负载在基底表面的氧化钌(RuO2)。所述基底为预处理过的钛箔,将含有水合氯化钌、盐酸的正丁醇溶液滴涂在预处理过的钛箔表面,所得钛箔负载的含钌的前驱体聚合物在烘箱中固化后在马弗炉中高温煅烧,得到钛箔负载氧化钌电极材料。所述电极材料具有良好的电催化活性,将其应用于电催化氧化氨氮反应,可以达到良好的氨氮去除效果并实现较高的氮气选择性。所述电极材料催化活性高,电氯化性能好,氮气选择性高。
Description
技术领域
本发明属于电催化技术领域,具体涉及一种用于电催化氧化氨氮的电极及其制备方法和应用。
背景技术
工业、农业和生活废水的大量排放,不可避免的会直接或间接的产生大量的氨氮污染从而导致水体富营养化,对水质造成严重影响。
为了减弱氨氮的危害亟需寻找一种合适的氨氮去除方法,传统的去除氨氮的方法包括生物法,吹脱法,化学沉淀法,折点氯化法,膜分离,离子交换法等等,但是由于成本高,副产物多以及反应速率低等限制不适用于大规模的应用。所以需要找到一种更加合适的去除方式,相比之下,电催化氧化氨氮由于条件温和,选择性好等特点逐渐发展起来。电催化氧化氨氮是利用阳极进行氧化,但是由于电极本身的氧化能力有限,因此通常使用电氯化辅助的方式来提高氨氮的电催化氧化效果。
本发明提供了一种钛箔负载氧化钌电极材料的制备方法,并应用于水体中氨氮的电催化氧化中。
发明内容
为实现氨氮的高去除率和高氮气选择性,本发明目的在于提供一种用于电催化氧化氨氮的电极。
本发明的再一目的在于:提供一种上述用于电催化氧化氨氮的电极产品的制备方法。
本发明的又一目的在于:提供一种上述产品的应用。
本发明目的通过下述方案实现:一种用于电催化氧化氨氮的电极,是一种钛箔负载氧化钌的电极材料,所述电极材料包括基底和负载在基底表面的氧化钌纳米颗粒(RuO2);所述基底为经预处理的钛箔。
在上述方案基础上,所述的预处理的钛箔为:钛箔依次经过丙酮和氢氧化钠溶液浸泡后在盐酸中加热,然后用超纯水和乙醇洗涤后备用。
进一步的,所述预处理具体包括:将钛箔置于丙酮中进行浸洗15 min,超声洗涤5min;用超纯水冲洗后,采用氢氧化钠浸泡1 h,超声5 min;用超纯水洗涤后在盐酸中加热浸泡2 h,用超纯水和乙醇冲洗备用。
较优的,所述氢氧化钠溶液的质量分数为30% ~ 60%;所述盐酸浓度为6 M ~ 8 M,所述在盐酸中加热浸泡温度为70℃ ~ 95℃。
本发明提供一种用于电催化氧化氨氮的电极的制备方法,其特征在于,所述方法包括以下步骤:
(1)将0.778 g RuCl3•xH2O溶于0.5 ml盐酸和4.5 ml正丁醇中,搅拌20 min~ 40min得到前驱体溶液;
(2)取一滴步骤(1)得到的前驱体溶液均匀滴涂在预处理过的钛箔表面,100℃ ~120℃烘干10 min ~ 20 min,然后以2℃/min ~6℃/min升温速率在450℃焙烧20 min,重复上述步骤两次,最后在450℃焙烧2 h,即得所述钛箔负载氧化钌电极材料(RuO2/Ti)。
作为本发明的一个实施方案,所述固化温度为100℃ ~ 120℃。优选所述固化温度为100℃。
作为本发明的一个实施方案,所述煅烧升温速率为2℃/min ~ 6℃/min。优选所述升温速率为4℃/min。
本发明提供一种用于电催化氧化氨氮的电极在电催化氧化氨氮的应用。
该钛箔负载氧化钌电极材料是一种电催化活性高,氮气选择性高的电极材料。本发明利用热涂覆分解法将氧化钌直接负载在钛箔表面。
本发明所述的钛箔负载氧化钌电极材料,是采用预处理的钛箔作为基底,利用热涂覆分解法将氧化钌直接生长在钛箔表面,即得到高催化活性高选择性的电催化电极材料。与现有技术相比,本发明具有如下的有益效果:
1)采用热涂覆分解法使氧化钌纳米颗粒直接生长在钛箔表面,电极制备方式简单,导电性良好,有利于大规模实际应用。
2)本发明的钛箔负载氧化钌电极材料催化活性高,氮气选择性好,解决了传统电极材料催化活性差,选择性低等问题。
附图说明
通过阅读参照以下附图对非限制性实施例和对比例所作的详细描述,本发明的其它特征、目的和优点将会变得更明显:
图1为RuO2/Ti电极的扫描电镜图;
图2为RuO2/Ti电极的X射线衍射图;
图3为RuO2/Ti电极电催化氧化氨氮的性能图。
具体实施方式
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明,但不以任何形式限制本发明。应当指出的是,对本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进。这些都属于本发明的保护范围。
实施例1
一种用于电催化氧化氨氮的电极,是一种钛箔负载氧化钌的电极材料RuO2/Ti,包括基底和负载在基底表面的氧化钌纳米颗粒;所述基底为经预处理的钛箔;按下述步骤制备:
(1)将剪成2 cm * 2.5 cm的钛箔放置在丙酮中进行浸洗15 min,超声洗涤5 min;用超纯水冲洗后,采用40%氢氧化钠浸泡1 h,超声5 min;用超纯水洗涤后在6 M盐酸中80℃加热浸泡2 h,用超纯水和乙醇冲洗得到预处理的钛箔,备用;
(2)将0.778 g RuCl3•xH2O溶于0.5 ml盐酸和4.5 ml正丁醇中,搅拌20 min得到前驱体溶液;
(3)取一滴步骤(2)得到的前驱体溶液均匀滴涂在预处理过的钛箔表面,100℃烘干10 min固化,然后以4℃/min升温速率在450℃焙烧20 min,重复上述步骤两次,最后在450℃焙烧2 h,即得所述钛箔负载氧化钌电极材料RuO2/Ti。
将得到的钛箔负载氧化钌电极材料RuO2/Ti进行形貌表征,如图1所示和X射线衍射分析,如图2所示。
应用例1
在60 ml含50 mg/L NH4 +-N的硫酸铵溶液中加入0.05 mol/L硫酸钠和1 g/L NaCl。采用三电极体系,工作电极为本实施例制备的RuO2/Ti,对电极采用钛片电极,采用饱和甘汞电极作为参比电极,在3 V的电压下电解1.5 h后氨氮的去除率为100%,见图3所示,氮气选择性为94%。
应用例2
本应用例1不同之处在于电解液中不添加氯化钠。
在60 ml含50 mg/L NH4 +-N的硫酸铵溶液中加入0.05 mol/L硫酸钠。采用三电极体系,工作电极为制备的RuO2/Ti,对电极采用钛片电极,采用饱和甘汞电极作为参比电极,在3 V的电压下电解1.5 h,几乎没有氨氮去除,见图3所示。
Claims (8)
1.一种用于电催化氧化氨氮的电极,其特征在于,是一种钛箔负载氧化钌的电极材料RuO2/Ti,包括基底和负载在基底表面的氧化钌纳米颗粒;所述基底为经预处理的钛箔。
2.如权利要求1所述的用于电催化氧化氨氮的电极,其特征在于,所述预处理的钛箔为:钛箔依次经过丙酮和氢氧化钠溶液浸泡后在盐酸中加热,然后,用超纯水和乙醇洗涤后得到。
3.如权利要求2所述用于电催化氧化氨氮的电极,其特征在于,所述氢氧化钠溶液的质量分数为30% ~ 60%。
4.如权利要求2所述用于电催化氧化氨氮的电极,其特征在于,所述盐酸浓度为6 M ~8 M,加热温度为70℃ ~ 95℃。
5.一种如权利要求1-4中任一项所述用于电催化氧化氨氮的电极的制备方法,其特征在于,所述方法包括以下步骤:
(1)将0.778 g RuCl3•xH2O溶于0.5 ml盐酸和4.5 ml正丁醇中,搅拌20 min~ 40 min得到前驱体溶液;
(2)取一滴步骤(1)得到的前驱体溶液均匀滴涂在钛箔表面,100℃ ~ 120℃烘干10min ~ 20 min,然后以2℃/min ~6℃/min升温速率在450℃焙烧20 min,重复上述步骤两次,最后在450℃焙烧2 h,即得所述钛箔负载氧化钌电极材料RuO2/Ti。
6.如权利要求5所述用于电催化氧化氨氮的电极的制备方法,其特征在于,按以下步骤:
(1)将剪成2 cm * 2.5 cm的钛箔放置在丙酮中进行浸洗15 min,超声洗涤5 min;用超纯水冲洗后,采用40%氢氧化钠浸泡1 h,超声5 min;用超纯水洗涤后在6 M盐酸中80℃加热浸泡2 h,用超纯水和乙醇冲洗得到预处理的钛箔,备用;
(2)将0.778 g RuCl3•xH2O溶于0.5 ml盐酸和4.5 ml正丁醇中,搅拌20 min得到前驱体溶液;
(3)取一滴步骤(2)得到的前驱体溶液均匀滴涂在预处理过的钛箔表面,100℃烘干10min固化,然后以4℃/min升温速率在450℃焙烧20 min,重复上述步骤两次,最后在450℃焙烧2 h,即得所述钛箔负载氧化钌电极材料RuO2/Ti。
7.一种如权利要求1-4中任一项所述用于电催化氧化氨氮的电极在电催化氧化氨氮的应用。
8.如权利要求7所述用于电催化氧化氨氮的电极在电催化氧化氨氮的应用,其特征在于,采用下述步骤:
在60 ml含50 mg/L NH4 +-N的硫酸铵溶液中加入0.05 mol/L硫酸钠和1 g/L NaCl,采用三电极体系,工作电极为本实施例制备的RuO2/Ti,对电极采用钛片电极,采用饱和甘汞电极作为参比电极,在3 V的电压下电解1.5 h。
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