白云石均匀沉淀法和反相微乳液法制备纳米氧化镁的方法研究
发布时间：2018-11-11 16:08
【摘要】： 纳米氧化镁是一种新型高功能精细无机材料。其本身具有的量子尺寸效应,小尺寸效应,表面效应,宏观量子隧道效应等使其具有明显优于本体材料的性能。本文介绍了纳米氧化镁的国内外研究现状,探讨了均匀沉淀法以及微乳液法反应的原理,并采用白云石均匀沉淀法以及反相微乳液法制得了纳米氧化镁晶体。 本文直接以湖南永州市东安县白云石矿为镁源,采用均匀沉淀法制得了纳米氧化镁晶体,并且用正交试验等研究了制备粒径小、分散程度好的纳米氧化镁颗粒的最佳条件。用原子吸收(AAS)、X射线衍射(XRD)、扫描电镜(SEM)、热重分析(TGA)等方法对产物进行了表征和分析。研究了分散剂种类、分散剂用量、沉淀剂种类、溶剂等对纳米氧化镁粒径的影响,并应用相关理论对各因素造成的影响进行了机理探讨。这对纳米氧化镁的工业化制备具有一定的参考价值。 采用正交试验法确定了制备纳米氧化镁的最佳工艺条件为：以淀粉为分散剂,用量为45%(质量百分含量),以尿素为沉淀剂,在70℃下超声波20分钟,然后沉淀离心洗涤,真空常温干燥,灼烧。结果表明采用该法制备的纳米粒子分散性好,晶体粒子分布均匀,结晶度高,纳米颗粒粒径为12.5纳米,且粒子产率达到86%。该法制备纳米氧化镁,具有广泛的应用前景。 由于微乳液法制备纳米材料不仅可以实现粒径可控,而且可以实现形貌可控,它已成为合成纳米颗粒的一种有效方法,受到人们的青睐,但目前通过反相微乳液制备纳米MgO的文献很少。本工作采用反相胶团作为微反应器,使溶解在水核内的试剂在水核内发生反应,并研究了不同水相/表面活性剂质量比(w0),煅烧温度,反应物浓度,陈化时间,以及反应温度等对制备MgO纳米粒子的影响,表征了粒子的结构,并对其形成机理进行了探讨。 通过聚乙二醇辛基苯基醚(曲拉通X-100)/正丁醇/正庚烷/水溶液形成的反相微乳体系,合成了MgO纳米粒子。对前驱体进行热重分析(TGA),确定了合适的煅烧温度为600℃。采用X射线衍射(XRD)、扫描电镜(SEM)、紫外可见分光光度法(UV-vis)分别对产物的结构、粒度和形貌进行了表征,考察了微乳液中水与表面活性剂的质量比(w0)对纳米氧化镁紫外屏蔽性能的影响以及煅烧温度、反应物浓度、陈化时间、反应温度等关键因素对产物粒子尺寸形貌的影响,并通过分析进一步揭示了Mg0纳米粒子的形成机理。结果表明,控制w0为15,煅烧温度为600℃,反应物浓度为0.05mol/L,陈化时间为15小时且反应温度在30℃时可得到分散性好,粒径分布均匀的MgO纳米粒子。
[Abstract]:Nanometer magnesium oxide is a new high function fine inorganic material. The quantum size effect, the small size effect, the surface effect and the macroscopic quantum tunneling effect make it superior to the bulk material. This paper introduces the research status of nano-MgO at home and abroad, discusses the reaction principle of homogeneous precipitation method and microemulsion method, and uses dolomite homogeneous precipitation method and reverse microemulsion method to obtain nano-MgO crystal. In this paper, nanocrystalline magnesium oxide was prepared by homogeneous precipitation method with dolomite ore in Dongan County, Yongzhou City, Hunan Province as the source of magnesium. The optimum conditions for preparing nanometer magnesium oxide particles with small particle size and good dispersion degree were studied by orthogonal test. The products were characterized and analyzed by atomic absorption (AAS), X diffraction (AAS), X) (XRD), scanning electron microscopy (XRD),) (SEM), thermogravimetric analysis (TGA). The effects of dispersant, amount of dispersant, precipitator and solvent on the particle size of nano-MgO were studied. It has certain reference value for the industrial preparation of nanometer magnesium oxide. The optimum technological conditions for preparing nanometer magnesium oxide were determined by orthogonal test: starch as dispersant, dosage 45% (mass%), urea as precipitant, ultrasonic wave for 20 minutes at 70 鈩，
本文编号：2325390
[Abstract]:Nanometer magnesium oxide is a new high function fine inorganic material. The quantum size effect, the small size effect, the surface effect and the macroscopic quantum tunneling effect make it superior to the bulk material. This paper introduces the research status of nano-MgO at home and abroad, discusses the reaction principle of homogeneous precipitation method and microemulsion method, and uses dolomite homogeneous precipitation method and reverse microemulsion method to obtain nano-MgO crystal. In this paper, nanocrystalline magnesium oxide was prepared by homogeneous precipitation method with dolomite ore in Dongan County, Yongzhou City, Hunan Province as the source of magnesium. The optimum conditions for preparing nanometer magnesium oxide particles with small particle size and good dispersion degree were studied by orthogonal test. The products were characterized and analyzed by atomic absorption (AAS), X diffraction (AAS), X) (XRD), scanning electron microscopy (XRD),) (SEM), thermogravimetric analysis (TGA). The effects of dispersant, amount of dispersant, precipitator and solvent on the particle size of nano-MgO were studied. It has certain reference value for the industrial preparation of nanometer magnesium oxide. The optimum technological conditions for preparing nanometer magnesium oxide were determined by orthogonal test: starch as dispersant, dosage 45% (mass%), urea as precipitant, ultrasonic wave for 20 minutes at 70 鈩，
本文编号：2325390
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