CN116173988A - 一种二硫化钼-活性炭压电催化剂的制备及其应用 - Google Patents
一种二硫化钼-活性炭压电催化剂的制备及其应用 Download PDFInfo
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Abstract
本发明涉及高级氧化领域，具体涉及一种二硫化钼‑活性炭压电催化剂的制备及其应用。通过一步水热法制备了二硫化钼‑活性炭压电催化剂，该催化剂分散到水中后，通过施加连续超声振荡进行压电催化反应以产生活性氧物种。所述活性氧物种以过氧化氢、单线态氧和超氧阴离子的形式存在。产生的活性氧可以驱动水和污染物发生氧化还原反应，达到水体中污染物的有效去除。
Description
技术领域
本发明涉及高级氧化领域，具体涉及一种二硫化钼-活性炭压电催化剂的制备及应用。
背景技术
近年来，人类的生产生活活动不断地向水环境中释放了大量污染物，如抗生素、染料、农药和内分泌干扰物等，并由此对人体和生物体的健康带来潜在影响。各种水处理技术，如混凝、膜过滤、生物滤池和高级氧化等被用来净化污染水体。其中，高级氧化技术因产生强氧化性的活性氧(Reactive oxygen species，ROS)，如·OH、·O2 -、1O2和H2O2等，可以将水体中的污染物降解为无害的CO2和H2O而成为近年的研究热点。
作为高级氧化的一种，压电催化是指压电材料在机械力(如超声)的作用下发生变形，从而导致其表面的电子-空穴对分离，产生内建电场，驱动污染物和水发生氧化还原反应。过渡金属二硫化钼(奇数层)具有良好的压电效应，被广泛应用于水体中污染物的降解和水分解产氢。但是纯二硫化钼容易堆叠，会导致其压电催化效率的下降。
炭材料因其具有良好的导电性和化学稳定性，可以有效提升半导体的压电催化性能。将二硫化钼原位生长在活性炭上，不仅可以有效地阻止二硫化钼的堆叠，而且可以加速压电催化过程中的污染物的迁移和电子传输速率，有效地提高压电催化效率。同时，鉴于活性炭是工业化产物，二硫化钼和活性炭的耦合有利于压电催化剂的工业化拓展应用。
发明内容
针对纯二硫化钼压电催化过程中的堆叠问题，本发明提供一种二硫化钼-活性炭压电催化材料，可实现水体中污染物的高效降解，达到去除工业废水中污染物的目的。该催化剂制备方法简单、成本低廉，绿色环保且具有较高的稳定性。
为实现上述目的，本发明提供一种二硫化钼-活性炭压电催化剂的制备，包括以下步骤：
(1)将一定量的钼酸铵和硫脲溶解在60mL超纯水中，得到溶液A；
(2)将一定量的活性炭加入溶液A，得到溶液B；
(3)将溶液B超声处理30min，得到悬浮液C；
(4)将悬浮液C倒入100mL的聚四氟乙烯内衬的不锈钢高压釜中，该高压釜在一定温度下进行水热过程；
(5)将水热后的产物经过无水乙醇和超纯水的洗涤数次之后，于一定温度下过夜烘干得到二硫化钼-活性炭压电催化剂。
其中，步骤(1)中钼酸铵的质量为0.92-1.84g。
其中，步骤(1)中的硫脲的质量为1.22-2.44g。
进一步地，步骤(2)中的活性炭的质量为0.1-0.5g。
其中，步骤(3)中的超声条件为40kHz，功率为0-100W。
其中，步骤(4)中的水热温度范围为180-220℃。
其中，步骤(4)中的水热时间为18-24h。
其中，步骤(5)中的烘干温度为60-80℃。
进一步地，步骤(5)中的烘干时间为8-12h。
本发明制备的二硫化钼-活性炭压电催化剂主要应用于水体中污染物的去除。
本发明的优点如下：
(1)本发明中的二硫化钼-活性炭催化剂通过一步水热法制备，流程简单，绿色环保，不需要进一步地退火处理，便于工业化拓展；
(2)本发明创新性地将压电材料与炭材料耦合，有利于提升压电催化剂对污染物的去除率，从而提升压电催化剂的催化效率；
(3)本发明用途广泛，除了应用于压电催化领域，还可以广泛地应用于光催化领域、压电光催化领域、水分解制过氧化氢、水分解制氢等领域；
(4)本发明制备的二硫化钼-活性炭可以重复利用，具有高度稳定性和长久操作性。
综上所述，本发明利用活性炭大的比表面积和层次化的孔结构，在活性炭表面原位生长二硫化钼，不仅可以有效地阻止二硫化钼纳米花的堆叠，而且可以加速压电催化过程污染物的迁移和电子的传递运输，从而有效地提高压电催化的效率。
附图说明
图1为二硫化钼-活性炭压电催化剂的制备工艺流程图；
图2为二硫化钼-活性炭的扫描电镜图；
图3为实施例1中二硫化钼、活性炭和二硫化钼-活性炭的X射线衍射图；
图4为实施例1和2中四环素的降解图；
图5为实施例3、4、5和6中不同捕获剂的添加对催化剂降解四环素的降解图；
图6为实施例1中二硫化钼-活性炭催化剂降解四环素的循环稳定图；
图7新鲜和使用过的实施例1中的催化剂的XRD图。
具体实施方案
以下将结合附图，对本发明的具体实施例进行解释说明。在此需要说明的是，对下述实施方案中的说明用于帮助理解发明，但并不构成对本发明的限定。
下述实施例中的实验方法，如无特殊说明，均为常规方法。下述实施例中所用的试验材料，如无特殊说明，均为可通过常规的商业途径购买得到。
实施例1
根据图1的工艺流程图，本实施例1包括以下步骤：
(1)二硫化钼-活性炭压电催化剂的制备
称取0.92g钼酸铵和1.22g硫脲溶解于60mL超纯水中，搅拌使得钼酸铵和硫脲完全溶解。称取0.3g的活性炭，并将其加入上述钼酸铵和硫脲的混合溶液中。随后，该溶液置于超声清洗机中，超声30min，使得溶液中各组分完全混合。将该混合溶液倒入100mL的聚四氟乙烯内衬不锈钢高压釜中，随后将高压釜放入烘箱，在200℃下水热24h。将水热后的产物用无水乙醇和超纯水洗涤数次后，于烘箱中60℃过夜干燥得到二硫化钼-活性炭压电催化剂。
(2)以二硫化钼作为对照，其制备方法为：
称取0.92g钼酸铵和1.22g硫脲溶解于60mL超纯水中，搅拌使得钼酸铵和硫脲完全溶解。随后，该溶液置于超声清洗机中，超声30min，使得溶液中各组分完全混合。将该混合溶液倒入100mL的聚四氟乙烯内衬不锈钢高压釜中，随后将高压釜放入烘箱，在200℃下水热24h。将水热后的产物用无水乙醇和超纯水洗涤数次后，于烘箱中60℃过夜干燥得到二硫化钼-活性炭压电催化剂。
(3)压电催化四环素的降解
分别称取40mg的步骤(1)和步骤(2)中的压电催化剂，将其分别放入80mL的40mg/L的四环素溶液中，在暗处搅拌20min以达到吸附-脱附平衡，随后，置于超声下超声60min，在特定时间取出3mL的上清液，过0.45μm的滤头后测试上清液的浓度。经计算公式R＝(C-20-Ct)/C-20*100％(其中，R是溶液的四环素降解效率，C-20是四环素溶液初始浓度，Ct是溶液t时刻的四环素浓度)得到溶液中四环素的去除率。经分析计算(图1)，二硫化钼和二硫化钼-活性炭压电催化剂对四环素的去除率分别为62.53％和98.97％。
实施例2
与实施例1相比，区别在于：在制备过程中将活性炭的添加量改为0.2g，其他制备方法同实施例1。
应用方法同实施例1，实施例2中制备的二硫化钼-活性炭压电催化材料对四环素的去除率为95.74％。
实施例3
测试压电催化降解过程中的ROS，进行捕获实验，具体步骤如下：
称取40mg实施例1中的催化剂和2mL异丙醇，分散在80mL的40mg/L的四环素溶液中，在暗处搅拌20min以达到吸附-脱附平衡，随后，置于超声下超声60min，在特定时间取出3mL的上清液，过0.45μm的滤头后测试上清液的浓度。经分析计算，四环素的降解效率为98.53％。
实施例4
与实施例3相比，区别在于：在反应过程中不再加入异丙醇，改为加入0.022g的对苯醌，其它制备方法同实施例3。经分析计算，四环素的去除效率为93.04％。
实施例5
与实施例3相比，区别在于：在反应过程中不再加入异丙醇，改为加入0.001g的过氧化氢酶，其它制备方法同实施例3。经分析计算，四环素的去除效率为75.24％。
实施例6
与实施例3相比，区别在于：在反应过程中不再加入异丙醇，改为加入0.031g的L-组氨酸，其它制备方法同实施例3。经分析计算，四环素的去除效率为93.04％。
为了进一步验证二硫化钼-活性炭压电催化剂的可重复使用性和稳定性，测试了新鲜和使用过的实施例1中的催化剂的X射线衍射图进行比较。重复使用的催化剂和新鲜催化剂的X射线衍射图中的晶体结构没有明显差异，表明二硫化钼-活性炭压电催化剂具有良好的稳定性。
以上所述仅为本发明的优选实施方案，并不用于限制本发明。对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本实用发明的精神和原则之内，所做的任何修改、等同替换、改进等，均应包含在本发明的保护范围内。
Claims (7)
1.一种二硫化钼-活性炭压电催化材料在压电催化中的应用，其特征在于：利用一步水热法制备二硫化钼-活性炭压电催化剂，并将其分散在含有污染物的溶液中，进行水体中污染物的有效去除。
2.根据权利要求1所述的一种二硫化钼-活性炭压电催化材料在压电催化中的应用，其特征在于：一步水热法制备二硫化钼-活性炭压电催化材料，包括以下步骤：
将一定量的钼酸铵和硫脲充分溶解到超纯水中，然后将一定量的活性炭加入上述溶液中，超声30min形成悬浮液；该悬浮液倒入100mL的聚四氟乙烯内衬不锈钢高压釜中，该高压釜在一定温度下进行水热过程；随后将水热后的产物进行过滤，干燥得到二硫化钼-活性炭压电催化剂。
3.根据权利要求2所述的一步水热法制备二硫化钼-活性炭压电催化材料，其特征在于：钼酸铵的质量为0.92-1.84g；硫脲的质量为1.22-2.44g；活性炭的质量为0.1-0.3g。
4.根据权利要求2所述的一步水热法制备二硫化钼-活性炭压电催化材料，其特征在于：超声条件为40kHz，功率为0-100W。
5.根据权利要求2所述的一步水热法制备二硫化钼-活性炭压电催化材料，其特征在于：水热温度为180-220℃，水热时间为18-24h。
6.根据权利要求2所述的一步水热法制备二硫化钼-活性炭压电催化材料，其特征在于：烘干温度为60-80℃，烘干时间为8-12h。
7.根据权利要求1-6所述的一种二硫化钼-活性炭压电催化材料在压电催化中的应用，其特征在于：所述压电催化反应在超声条件下暗处进行。
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