二硫化鉬的水熱制備及其光催化降解性能研究
發(fā)布時間:2018-04-22 00:29
本文選題:二硫化鉬 + 水熱法。 參考:《沈陽師范大學(xué)》2017年碩士論文
【摘要】:二硫化鉬(MoS2)為輝鉬礦的主要成分,與石墨烯具有相同的層狀結(jié)構(gòu)。二硫化鉬納米材料應(yīng)用比較廣泛,摩擦學(xué)領(lǐng)域、電化學(xué)領(lǐng)域等均有涉及。二硫化鉬擁有1.78 eV的能帶隙,并比表面積大,因此,在可見光催化領(lǐng)域具有廣泛的應(yīng)用前景。目前,制備二硫化鉬的方法種類繁多,如利用機械剝離法制備單層二硫化鉬,利用氣相沉積法制備形貌各異的二硫化鉬粉體,利用水熱法制備不同尺寸的二硫化鉬。但是,二硫化鉬粉體的分散性較差,太陽光利用波段偏窄,在制氫等特定光催化領(lǐng)域可見光光催化效率偏低。如果制備二硫化鉬過程中通過親水性有機修飾,阻止粒子間團(tuán)聚,形成可溶性二硫化鉬膠體,并在表面負(fù)載光敏化劑拓展太陽光利用波段,可有效提高二硫化鉬的光催化性能。本文采用二步水熱法制備膠體二硫化鉬,以鉬酸銨和硫脲分別作為鉬源和硫源,制備甲脒基硫代鉬前驅(qū)體,水合肼還原前驅(qū)體,制備甲瞇基二硫化鉬膠體。制備過程中,利用紫外光譜和熒光光譜分析,分別考察了水熱反應(yīng)溫度、水熱反應(yīng)時間、物料比對前驅(qū)體制備和二硫化鉬膠體制備的影響。確定前驅(qū)體制備的最佳反應(yīng)溫度140℃、反應(yīng)時間24 h、鉬硫比1:4;還原前驅(qū)體制備二硫化鉬的最佳反應(yīng)溫度100℃、反應(yīng)時間4 h、鉬氮比1:12。最后,利用三聯(lián)吡啶氯化釕光敏化劑對膠體二硫化鉬進(jìn)行光敏化。為了考察所制備的膠體二硫化鉬的光催化性能和光敏化效果,以考馬斯亮藍(lán)為光催化降解對象,進(jìn)行了可見光催化降解實驗。實驗結(jié)果表明,三聯(lián)吡啶氯化釕光敏化甲瞇基二硫化鉬膠體的可見光光催化效果顯著。光催化效率與光敏化劑負(fù)載濃度、催化劑用量及光照強度均相關(guān),光催化效率隨著催化劑用量、光照強度及負(fù)載濃度的增加而逐漸提高,但是負(fù)載濃度過高時催化效率反而降低。
[Abstract]:Molybdenum disulfide (MoS _ 2) is the main component of molybdenum and has the same layered structure as graphene. Molybdenum disulfide nanomaterials are widely used in tribology and electrochemistry. Molybdenum disulfide has an energy band gap of 1.78 EV and a large specific surface area. Therefore, molybdenum disulfide has a wide application prospect in visible light catalysis. At present, there are many methods to prepare molybdenum disulfide, such as the preparation of monolayer molybdenum disulfide by mechanical stripping, the preparation of molybdenum disulfide powder with different morphologies by vapor deposition, and the preparation of molybdenum disulfide of different sizes by hydrothermal method. However, the dispersion of molybdenum disulfide powder is poor, the utilization band of solar light is narrow, and the visible photocatalytic efficiency is low in the specific photocatalytic field such as hydrogen production. If molybdenum disulfide was modified by hydrophilic organic modification to prevent the agglomeration between particles and form soluble molybdenum disulfide colloid, the photocatalytic activity of molybdenum disulfide could be improved effectively if the surface loaded Guang Min was used to expand the band of solar light. In this paper, the colloidal molybdenum disulfide was prepared by two-step hydrothermal method. Ammonium molybdate and thiourea were used as molybdenum source and thiourea, respectively, to prepare formamidine thio molybdenum precursor. Hydrazine hydrate was used to reduce the precursor to prepare molybdenum methylene disulfide colloid. The effects of hydrothermal reaction temperature, hydrothermal reaction time, material ratio on preparation of precursor and preparation of molybdenum disulfide colloid were investigated by UV and fluorescence spectra, respectively. The optimum reaction temperature of the precursor was 140 鈩,
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