CN113463126A - 一种非贵金属析氯催化剂电极及制备方法 - Google Patents
一种非贵金属析氯催化剂电极及制备方法 Download PDFInfo
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Abstract
本发明属于海洋污损防护技术领域，具体涉及一种非贵金属析氯催化剂电极及制备方法。非贵金属析氯催化剂电极，包括基体，所述基体表面沉积催化剂Co(OH)2。本发明负载电解海水析氯的非贵金属催化剂的电极可以显著提高电解海水的效率，并且可以在短时间、小电压的通电情况下产生足量且可控制的具有生物杀灭作用的有效氯，从而达到防污的效果。
Description
技术领域
本发明属于海洋污损防护技术领域，具体涉及一种非贵金属析氯催化剂电极及制备方法。
背景技术
海洋生物污损问题是一个长期困扰人类的问题，它给海洋探索过程中使用的各种设备带来了诸多的负面影响，例如降低船舶航行速度、堵塞冷却水通道以及影响水下传感器数据收集的准确性。这也刺激了人们对海洋设备的防污损技术的开发。目前，市场上用于防污的手段主要有以下三种：（1）纯粹的机械设备，例如刮刀；（2）基于铜和三丁基锡生物杀灭剂浸出系统；（3）基于局部电解海水活性氯生成的生物杀灭剂生成系统。机械防污在进行几个操作周期以后需要人工维护，不适合远程设备的使用。三丁基锡防污具有长效性，但是对海洋环境有巨大的危害。电化学氯化局部生成生物杀灭剂因其操作简单、可控性强成为最有前景的海洋防污技术。
电解海水制氯关键的就是电解析氯所用的阳极材料。而电解海水与氯碱工业的电解产氯技术不同，电解海水过程中氯离子浓度低，且作为电解质的海水呈现近中性，使得在电解的过程中不仅有析氯反应，同时还伴随着大量的析氧反应。目前成熟的商业级析氯电极-DSA电极仅仅解决了电解高浓度氯离子的问题，对于电解海水还存在低选择性和低稳定性等问题。此外，目前针对电解海水析氯的催化剂大多都还是基于贵金属及其氧化物的研究，由于高成本使得其应用受限。
因此，开发低成本、高活性的电解海水析氯催化剂有助于进一步推动电解海水析氯技术在海洋防污方向的应用。
发明内容
本发明的目的是提供一种具有优异析氯性能的非贵金属析氯催化剂电极及制备方法，以解决现有析氯电极存在的问题和缺陷。
为了实现上述目的，本发明提供的其中一种技术方案为：一种非贵金属析氯催化剂电极，包括基体，所述基体表面沉积有Co(OH)2催化剂。
作为本发明的一种优选方式，所述的基体为金属钛。
为了实现本发明的目的，本发明还提供了上述非贵金属析氯催化剂电极的制备方法，该方法包括：
在Co(NO3)2溶液中，采用阴极恒电压法在基体表面制备析氯催化剂Co(OH)2，得到催化剂电极；
采用线性伏安扫描法对所述基体表面的催化剂进行活化处理。
进一步优选地，所述阴极恒电压法实现的温度为0~50℃，电沉积时间为10s~900s。
进一步优选地，线性伏安扫描的电压为0.55~1.55 V。
本发明还提供上述非贵金属析氯催化剂电极的应用，所述催化剂电极作为阳极，其作为催化剂阳极电解海水制氯，用于水下光学窗口防污。
与现有技术相比，本发明具有如下有益效果：
本发明负载电解海水析氯的非贵金属催化剂的电极可以显著提高电解海水的效率，并且可以在短时间、小电压的通电情况下产生足量且可控制的具有生物杀灭作用的有效氯，从而达到防污的效果。本发明的非贵金属析氯催化剂电极的制备过程简单，并且通过对催化剂的活化处理，提高其电催化活性，制备方法所使用的实验的仪器和药品也容易获得，对环境无危害。
附图说明
图1为实例1方法制备的钴基薄膜催化剂的X射线衍射图（XRD）；
图2为实例1方法制备的钴基薄膜催化剂的扫描电镜图（SEM）；（a）活化处理前；（b）活化处理后；
图3为实例1方法制备的钴基薄膜催化剂在3.5% NaCl 和中性饱和NaCl溶液中的线性扫描曲线，扫描速率10 mV/s；
图4为实例1方法制备的钴基薄膜催化剂电极和商用析氯电极DSA在3.5% NaCl 溶液中的线性扫描曲线，扫描速率10 mV/s；
图5为实例1方法制备的钴基薄膜催化剂的稳定性测试图。
具体实施方式
为了便于理解本发明，下面结合附图和具体实施例，对本发明进行更详细的说明。附图中给出了本发明的较佳的实施例。但是，本发明可以以许多不同的形式来实现，并不限于本说明书所描述的实施例。相反地，提供这些实施例的目的是使对本发明公开内容的理解更加透彻全面。
实施例1 本实施例提供的非贵金属析氯催化剂电极，主要由括钛网和钛网表面的薄膜催化剂Co(OH)2构成。
本实施例的非贵金属析氯催化剂电极，采用阴极恒电压电沉积法制备，具体包括以下步骤：
（1）将纯度为99.99%的钛网按1cm×1cm进行切割，用蒸馏水冲洗钛网的表面。冲洗干净以后，用无水乙醇对其进行超声清洗20 min，清洗结束后将无水乙醇倒掉换成蒸馏水进行20 min的超声清洗，清洗完毕后放入60 ℃的烘箱中使其表面快速干燥。
（2）将处理好的钛网用电极夹夹好，作为工作电极，另外铂网和饱和甘汞电极分别作为对电极和参比电极，将其放入25℃ 60 mL 0.1M Co(NO3)2溶液中，在电极间施加-1 V（vs. SCE）的恒定电压，维持850s，停止后取下工作电极，在室温下干燥，所制得的Co(OH)2析氯催化剂负载在钛网上。
（3）将上述制得的电极作为工作电极，铂网和饱和甘汞电极张分别作为对电极和参比电极，放入60 mL 3.5% NaCl 溶液中，在室温下进行线性扫描，扫描速率为10 mV/s，从0.55 V（vs. SCE）开始扫到1.55 V（vs. SCE）停止，取出电极室温下干燥，完成催化剂活化。
对本实施例制备的催化剂电极进行X射线衍射测定，如图1所示，根据XRD图可以确定所制备的析氯催化剂的主要成分是Co(OH)2。
图2 为本实施例制备的Co(OH)2电解海水析氯催化剂的SEM图。根据SEM图可以清楚的看出，Co(OH)2析氯催化剂电极表面呈现多层的纳米片结构，而且在活化处理前表面的纳米片较为团聚密集，而在活化处理之后催化剂表面微结构变得较为疏松，这无疑使得比表面积增大，从而其电催化活性也增大。另外，经过电化学氧化的纳米片厚度增大，其结构变得更加的稳定。
本对实施例制备的催化剂电极的电催化活性进行测试：
对比例采用以Co3O4为催化剂的电极。图3 为本实施例制备的Co(OH)2薄膜催化剂电极与Co3O4电极（Co3O4电极参照专利公开文献202110050042.6中的方法制备）分别在3.5%NaCl和饱和NaCl溶液中的线性扫描曲线，从曲线中可以看出，无论是在低浓度还是高浓度的NaCl溶液中，本实施制备的Co(OH)2薄膜催化剂具有优异的电催化活性，且均优于对比例的Co3O4电极。
图4为本实施例制备的Co(OH)2电解海水析氯催化剂阳极和商用析氯电极DSA在3.5% NaCl溶液中的线性扫描曲线，可以看出本实施例所制备Co(OH)2薄膜催化剂电极电解海水析氯性能优于商用DSA电极。
图5 为本实施例制备的Co(OH)2电解海水析氯催化剂在3.5% NaCl溶液中的稳定性测试，从图中曲线可以看出，所制备的非贵金属催化剂Co(OH)2具有优异的稳定性。
实施例2 本实施例提供的非贵金属析氯催化剂电极，主要由括钛片和钛片表面的薄膜催化剂Co(OH)2构成。
本实施例的非贵金属析氯催化剂电极，采用阴极恒电压电沉积法制备，具体包括以下步骤：
（1）将钛片按1cm×1cm进行切割，用蒸馏水冲洗钛片的表面。冲洗干净以后，用无水乙醇对其进行超声清洗20 min，清洗结束后将无水乙醇倒掉换成蒸馏水进行20 min的超声清洗，清洗完毕后放入60 ℃的烘箱中使其表面快速干燥。
（2）将处理好的钛片用电极夹夹好，作为工作电极，另外铂网和饱和甘汞电极分别作为对电极和参比电极，将其放入50℃ 60 mL 0.1M Co(NO3)2溶液中，在电极间施加-1 V（vs. SCE）的恒定电压，维持400s，停止后取下工作电极，在室温下干燥，所制得的Co(OH)2析氯催化剂负载在钛片上。
（3）将上述制得的电极作为工作电极，铂网和饱和甘汞电极张分别作为对电极和参比电极，放入60 mL 3.5% NaCl 溶液中在室温下进行线性扫描，扫描速率为10 mV/s，从0.55 V（vs. SCE）开始扫到1.55 V（vs. SCE）停止，取出电极室温下干燥，完成催化剂活化。
实施例3 本实施例提供的非贵金属析氯催化剂电极，主要由钛片和钛片表面的催化剂Co(OH)2构成。
本实施例的非贵金属析氯催化剂电极，采用阴极恒电压电沉积法制备，具体包括以下步骤：
（1）将钛片按1cm×1cm进行切割，用蒸馏水冲洗钛片的表面。冲洗干净以后，用无水乙醇对其进行超声清洗20 min，清洗结束后将无水乙醇倒掉换成蒸馏水进行20 min的超声清洗，清洗完毕后放入60 ℃的烘箱中使其表面快速干燥。
（2）将处理好的钛片用电极夹夹好，作为工作电极，另外铂网和饱和甘汞电极分别作为对电极和参比电极，将其放入25℃ 60 mL 0.1M Co(NO3)2溶液中，在电极间施加-1 V（vs. SCE）的恒定电压，维持600s，停止后取下工作电极，在室温下干燥，所制得的Co(OH)2析氯催化剂负载在钛片上。
（3）将上述制得的电极作为工作电极，铂网和饱和甘汞电极张分别作为对电极和参比电极，放入60 mL 3.5% NaCl 溶液中在室温下进行线性扫描，扫描速率为10 mV/s，从0.55 V（vs. SCE）开始扫到1.55 V（vs. SCE）停止，取出电极室温下干燥，完成催化剂活化。
Claims (6)
1.一种非贵金属析氯催化剂电极，包括基体，其特征在于：所述基体表面沉积有催化剂Co(OH)2。
2.根据权利要求1所述的非贵金属析氯催化剂电极，其特征在于：所述的基体为金属钛。
3.一种如权利要求1或2所述的非贵金属析氯催化剂电极的制备方法，其特征在于：在Co(NO3)2溶液中，采用阴极恒电压法在基体表面制备析氯催化剂Co(OH)2，得到催化剂电极；
采用线性伏安扫描法对所述基体表面的催化剂进行活化处理。
4.根据权利要求3所述的非贵金属析氯催化剂电极的制备方法，其特征在于：所述阴极恒电压法实现的温度为0~50℃，电沉积时间为10s~900s。
5.根据权利要求3所述的非贵金属析氯催化剂电极的制备方法，其特征在于：线性伏安扫描的电压范围为0.55~1.55 V。
6.一种如权利要求1或2所述的非贵金属析氯催化剂电极的应用，其特征在于：其作为催化剂阳极电解海水制氯，用于水下光学窗口防污。
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