CN113952961A - 一种新型镍钼合金纳米颗粒的制备方法及其处理废水的方法 - Google Patents
一种新型镍钼合金纳米颗粒的制备方法及其处理废水的方法 Download PDFInfo
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Abstract
本发明公开了一种新型镍钼合金纳米颗粒的制备方法及其处理废水的方法，包括如下步骤（1）MoNiOx/CNT的制备：（2）MoNi/CNT纳米结构的制备。通过本发明所述方法制备得到的镍钼合金纳米颗粒具有较高的电催化性能，Mo‑Ni合金形成后，Ni与Mo两种元素产生协同作用，有利于降低析氧电位，利于羟基自由基的产生，同时，在高电流密度电解下，Mo存在溶出效应，可以形成多孔结构，使电极的真实表面积增大，进一步提升镍钼合金纳米颗粒的电催化效果。
Description
技术领域
本发明涉及污水处理技术领域，具体涉及一种新型镍钼合金纳米颗粒的制备方法及其处理废水的方法。
背景技术
随着现代工业的日益发展，工业用水量及废水的排放量日益增加，世界各国的水体都出现了不同程度的污染，导致世界性的水资源匮乏危机日益严重。为极大地缓解水资源的短缺状况，工业废水处理技术的研究也日益受到人们的密切关注。
目前，已经开发了许多方法来处理废水，包括物理、化学或生物过程。尽管生物处理是一种低成本的技术，但由于废水特性的变化、高化学需氧量 (COD) 浓度和低生物降解性，生物处理系统可能无法持续达到处理要求。而物理和化学方法，例如离子交换、吸附和凝聚，只是将污染物转移到另一相而不是破坏它们。近年来，电化学氧化方法因其高效、易于操作和环境兼容性等优点而备受关注并开始替代传统工艺。
在污染物降解方面，电化学氧化是直接或间接通过在电极表面形成高氧化活性氧(•OH) 来氧化污染物的过程。通常，电化学氧化过程取决于阳极材料。铂、碳 、掺硼金刚石(BDD) 和金属氧化物都可用作阳极材料。其中，二氧化铅（PbO2 ）被广泛研究用于污水电化学氧化处理的阳极，但是PbO2 电极不稳定，Pb2+的析出会造成二次污染。因此，电催化处理废水技术推广受到电催化氧化催化剂的限制。
发明内容
针对现有技术存在的上述不足，本发明的目的在于提供一种用于废水电催化氧化裂解的镍钼合金纳米颗粒的制备方法，以解决现有技术通过水电解析氢催化剂成本高、稳定性差和二次污染等问题。
为了解决上述技术问题，本发明采用如下技术方案：
一种用于废水电催化氧化裂解的镍钼合金纳米颗粒的制备方法，包括如下步骤：
（1）MoNiOX/CNT的制备：
将碳管与乙二醇混合后，再加入Mo(CO)6和Ni(OAc)2，在150℃~200℃的条件下搅拌反应2~4h，反应结束后冷却至室温，洗涤多次后得到产物MoNiOX/CNT；其中，碳管、Mo(CO)6和Ni(OAc)2的质量比为1：(5~10)：(5~10)；
（2）MoNi/CNT纳米结构的制备：
将MoNiOX/CNT平铺在磁舟中，将所述磁舟放入管式炉中加热，待管式炉中空气排出后，在H2/Ar氛围中加热至450℃~550℃并保持反应20min~1h，得到产品MoNi/CNT。
本发明还提供一种利用镍钼合金纳米颗粒电催化氧化裂解处理废水的方法，采用如本发明所述制备方法制备得到所述镍钼合金纳米颗粒，将所述镍钼合金纳米颗粒与乙醇、水和Nafion配置成混合溶液，将所述混合溶液涂在碳电极表面后干燥，重复操作至少四次，以所述碳电极为阳极，碳棒为阴极，在污水中添加硫酸钠作为支持电解质，将阳极和阴极放在电解槽中进行裂解处理。
与现有技术相比，本发明具有如下有益效果：
1、通过本发明所述方法制备得到的镍钼合金纳米颗粒具有较高的电催化性能，Mo-Ni合金形成后，Ni与Mo两种元素产生协同作用，有利于降低析氧电位，从而提高氧化裂解效率，同时，在高电流密度电解下，Mo存在溶出效应，可以形成多孔结构，使电极的真实表面积增大，进一步提升镍钼合金纳米颗粒的催化效果。
2、本发明利用在电极表面形成的高度氧化自由基（·OH）对污水中的有机物进行氧化，高度氧化的自由基能够与有机物发生碰撞，导致共价键断裂并与·OOH 反应，而且，随着降解时间的延长，产生的化合物进一步与·OH碰撞并产生新的中间体，新的中间体最终可以被裂解成水和二氧化碳，从而达到处理和降解水中有机污染物的目的。
附图说明
图1为实施例1的MoNi/CNT纳米材料的XRD图。
图2为生长在CNT上的实施例1的MoNi合金纳米颗粒的TEM图。
图3为电催化裂解的H型电解槽示意图。
具体实施方式
下面将结合附图和实施例对本发明作进一步说明。
一、新型镍钼合金纳米颗粒的制备
（1）MoNiOX/CNT的制备：
将20mg碳管与60ml乙二醇混合，并超声处理1h后使其分散均匀。将其加入100ml圆底烧瓶中，再加入150mg的Mo(CO)6和100mg的Ni(OAc)2，在190℃的条件下，以1500r/min的搅拌速度反应3h，反应结束后冷却至室温，用超纯水洗涤多次后得到产物MoNiOX/CNT。
（2）MoNi/CNT纳米结构的制备：
将30mg的MoNiOX/CNT平铺在磁舟中，将所述磁舟放入管式炉中加热，待管式炉中空气排出后，在H2/Ar氛围中加热至500℃并保持反应30min，得到产品MoNi/CNT。
根据表1的原料配比，采用上述方法制备实施例1~5。
表1
| 实施例 | 碳管、Mo(CO)<sub>6</sub>和Ni(OAc)<sub>2</sub>的质量比 | 反应温度（℃） | 产品形貌 |
| 1 | 1:2.5:5 | 500 | 纳米颗粒 |
| 2 | 1:5:5 | 500 | 纳米颗粒 |
| 3 | 1:5:5 | 600 | 纳米颗粒 |
| 4 | 1:5:7.5 | 500 | 纳米颗粒 |
| 5 | 1:5:10 | 500 | 纳米颗粒 |
二、一种利用镍钼合金纳米颗粒电催化氧化裂解处理废水的方法
采用实施例1~5和对比例1~2，将1mg镍钼合金纳米颗粒与50μL乙醇、190μL水和10μL的Nafion配置成混合溶液，超声处理至少40min形成均匀的分散体系。然后取25ul催化剂滴到在表面积为0.5cm2的碳纸电极上，所制备的催化剂膜在红外灯下干燥，重复滴四次。以亚甲基蓝有机污水为样本，添加少量Na2SO4作为支持电解质，以制备的电极为阳极，碳棒为阴极，在H型电解槽进行裂解反应。
以0.5 mol/L的亚甲基蓝为例，降解效果如表2所示。
表2
| 实施例 | 样品制备配比 | 样品制备反应温度（℃） | 电流密度（mA/cm<sup>-2</sup>） | 电解时间（min） | 亚甲基蓝去除率（%） | 法拉第效率（%） |
| 1 | 1:2.5:5 | 500 | 5 | 10 | 35.1 | 81.0 |
| 2 | 1:5:5 | 500 | 10 | 20 | 62.9 | 82.3 |
| 3 | 1:5:5 | 600 | 25 | 30 | 89.7 | 85.2 |
| 4 | 1:5:7.5 | 500 | 50 | 60 | 92.6 | 75.3 |
| 5 | 1:5:10 | 500 | 100 | 90 | 98.5 | 63.9 |
碳管、Mo(CO)6和Ni(OAc)2的质量比1:5:5，600℃条件下制备的样品，在电流密度为25mA/cm-2时，电解时间为30min，亚甲基蓝的去除率可达到89.7%，法拉第效率可达到85.2%。
三、稳定性测试
对实施例1~5进行稳定性测试，设置电流密度为25mA/cm-2，在20h的长时间裂解下，电流密度基本没有衰减，表明实施例1~5具有很好的稳定性。
最后需要说明的是，以上实施例仅用以说明本发明的技术方案而非限制技术方案，本领域的普通技术人员应当理解，那些对本发明的技术方案进行修改或者等同替换，而不脱离本技术方案的宗旨和范围，均应涵盖在本发明的权利要求范围当中。
Claims (7)
1.一种新型镍钼合金纳米颗粒的制备方法，其特征在于，包括如下步骤：
（1）MoNiOX/CNT的制备：
将碳管与乙二醇混合后，再加入Mo(CO)6和Ni(OAc)2，在150℃~200℃的条件下搅拌反应2~4h，反应结束后冷却至室温，洗涤多次后得到产物MoNiOX/CNT；其中，碳管、Mo(CO)6和Ni(OAc)2的质量比为1：(5~10)：(5~10)；
（2）MoNi/CNT纳米结构的制备：
将MoNiOX/CNT平铺在磁舟中，将所述磁舟放入管式炉中加热，待管式炉中空气排出后，在H2/Ar氛围中加热至450℃~550℃并保持反应20min~1h，得到产品MoNi/CNT。
2.根据权利要求1所述新型镍钼合金纳米颗粒的制备方法，其特征在于，在（1）中，碳管与乙二醇的质量比为1：(3~5)。
3.根据权利要求1所述新型镍钼合金纳米颗粒的制备方法，其特征在于，在（1）中，对混合后的碳管和乙二醇进行超声处理，使其分散均匀。
4.根据权利要求1所述新型镍钼合金纳米颗粒的制备方法，其特征在于，在（2）中，H2和Ar之间的体积比为1:10。
5.一种利用镍钼合金纳米颗粒电催化氧化裂解处理废水的方法，其特征在于，采用如权利要求1~4任一所述制备方法制备得到所述镍钼合金纳米颗粒，将所述镍钼合金纳米颗粒与乙醇、水和Nafion配置成混合溶液，将所述混合溶液涂在碳电极表面后干燥，重复操作至少四次，以所述碳电极为阳极，碳棒为阴极，在污水中添加硫酸钠作为支持电解质，将阳极和阴极放在电解槽中进行裂解处理。
6.根据权利要求5所述利用镍钼合金纳米颗粒电催化氧化裂解处理废水的方法，其特征在于，所述混合溶液中，镍钼合金纳米颗粒的用量为2~5mg/mL。
7.根据权利要求5所述利用镍钼合金纳米颗粒电催化氧化裂解处理废水的方法，其特征在于，所述混合溶液中，水、乙醇和Nafion的体积比为5:19:1。
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