二硫化钼环境稳定性及废水处理应用研究

         二硫化钼（Molybdenum disulfide，MoS₂）是一种新兴的二维层状材料，由于具有优异的吸附性能和良好的光催化性能等性质，使其在环境领域内的应用得到广泛关注。然而材料在使用过程中不可避免地会释放到环境中，对生态环境造成潜在的威胁，因此研究 MoS₂进入环境体系后的环境行为是十分必要的。本论文从 MoS₂纳米材料的环境稳定性展开研究，重点研究 MoS₂在自然环境和高级氧化工艺中的稳定性，从而为二硫化钼在环境领域内的应用研究提供一定的理论支持。
        本论文研究了水热合成法制备的 MoS₂纳米材料在自然环境中的环境稳定性，通过测定反应过程中 Mo 的释放来定量 MoS₂发生氧化溶解的程度；结果表明氧气是 MoS₂发生氧化溶解的必备条件，光照和碱性条件可以促进MoS₂的氧化溶解，而不同的金属阳离子对 MoS₂环境稳定性的影响作用不同，并且 MoS₂物相含量分布和形貌等自身的性质也会影响其环境稳定性；然后通过 XPS 分析反应过程中 MoS₂物相含量的变化，并通过 SEM 和 TEM观测材料反应前后形貌的变化，发现 MoS₂纳米材料在自然环境中自身性质会发生改变。
        本论文也研究了采用化学剥离法制备的 MoS₂纳米片层材料在高级氧化处理工艺中的环境稳定性。通过自由基淬灭实验和 EPR 技术表明 MoS₂纳米片层材料可以激活过一硫酸盐（PMS）生成硫酸根自由基和羟基自由基；而过量的 MoS₂纳米片层材料能够淬灭生成的自由基从而抑制污染物橙黄Ⅱ（Orange Ⅱ，OⅡ）的降解；由于 2H-SL-MoS₂的化学稳定性和吸附性更好，使其对自由基的淬灭作用不如 1T-SL-MoS₂，从而提出了通过减少激活剂的氧化位点来抑制自由基淬灭作用从而提高污染物降解性能的方案，为激活剂的设计提供了一个方向。该研究发现 MoS₂纳米材料在基于 PMS 的高级氧化工艺中不具备环境稳定性的性质。
        考虑到纳米材料在氧化性环境体系中存在环境稳定性问题，而含铬电镀废水也是一个氧化性体系，无法避免 MoS₂自身消耗的问题，同时为了节约成本，本论文以 MoS₂粉末为研究对象，探究其处理含铬电镀废水的性能。从反应的 pH、温度和 MoS₂粉末投加量三个方面优化了反应条件；并建立了处理不同浓度 Cr(Ⅵ)的废水和 MoS₂粉末投加量之间的关系；同时研究了MoS₂粉末对模拟工业废水的处理性能，表明 MoS₂具有同时处理铬铜共存电镀废水的实际应用潜能。

Molybdenum disulfide (MoS₂) is an emerging two-dimensional layered material, which has attracted extensive attention in the field of environmental engineering due to its excellent adsorption and photocatalytic properties. However, materials will inevitably be released into the environment during application, causing potential threats to the ecological environment. Therefore, it is necessary to study the environmental behavior of MoS₂ after entering the environmental system. In this thesis, the environmental stability of MoS₂ nanomaterials in natural environment and advanced oxidation process (AOPs) was studied, providing theoretical basis for the application of MoS₂ in the environmental field.

In this thesis, the environmental stability of MoS₂ nanomaterials prepared by hydrothermal synthesis method in natural environment was studied. The release of Mo during reactions was measured to quantify the oxidation dissolution extent of MoS₂. The results showed that oxygen was a prerequisite for the oxidation dissolution of MoS₂, irradiation and alkaline conditions could accelerate the dissolution process, and different metal cations had different effects on the environmental stability of MoS₂. Meanwhile the phase content and morphology of MoS₂ also affected the environmental stability of MoS₂. XPS technology was implemented to analyze the phase alteration of MoS₂, and SEM and TEM were recorded to detect the morphology change of the material, demonstrating that the properties of MoS₂ nanomaterials would change in natural environment.

The environmental stability of MoS₂ nanosheets prepared by chemical exfoliation method in advanced oxidation process was also studied in this thesis. Sulfate radical and hydroxyl radical were detected as the primary reactive oxygen species in the activation reaction system by radical quenching experiments and EPR technology, demonstrating that PMS could be activated by MoS₂. However, excessive MoS₂ nanosheets could quench radicals and thus inhibit the degradation of orange Ⅱ (OⅡ). More importantly, owing to the better chemical stability and adsorption capability, 2H-SL-MoS₂ exhibited weaker quenching effect than 1T-SL-MOS₂. The protection of oxidation active sites proved to be a feasible way of suppressing ROS quenching effect to improve the degradation performance, and thus providing a new sight for the activator design. It was found that MoS₂ nanomaterials do not possess the property of environmental stability in PMS-AOPs.

Given the matter of nanomaterials’ environmental stability, the problem of consumption of MoS₂ nanomaterials in the oxidative system of chromium-containing electroplating wastewater can not be avoided, and treatment costs, this work takes MoS₂ powder as the research object to explore its treatment performance to chromium-containing electroplating wastewater. The reaction conditions were optimized from three aspects, including pH, temperature, and MoS₂ powder dosage. The relationship between Cr(Ⅵ) concentration in wastewater and MoS₂ powder dosage required was established. Furthermore, the treatment performance of MoS₂ powder on simulated industrial wastewater was studied, indicating that MoS₂ has the practical application potential in the treatment of chromium-copper electroplating wastewater.

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