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
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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。
Nano-MgO is a new type of high function fine inorganic material. Because of its quantum size effect, small-size effect, surface effect, macroscopic quantum tunneling effect, etc, it has a superior performance to the materials now existing.This paper introduced the current research status on nano-MgO,the theory of homogenous precipitation and micro-emulsion reaction.The nano-MgO crystal was made by the sluggish precipitation method from dolomite and reverse microemulsion method
In this paper,the dolomite which was native to Dongan Countr y, Yongzhou City of Hunan Province was used to make the nano-MgO by the homogenous precipitation method.And the orthogonal test methodused was used to find the optimum conditions under which the nana-MgO of small size and good dispersion could be obtained.The atomic absorption (AAS), X-ray diffraction (XRD),scanning electron microscopy (SEM) and thermogravimetric (TGA) were used to research the effect of dispersant types, dispersant dosage, precipitant types and solvent on the size of nano-MgO. A discussion was devoted to the mechanism of the impact of every factor with correlate theory. And the research could be usefull for the industrialization of nano-MgO.
The optimum technological conditions which was decided by the orthogonal test was:The optimum synthesis condition of nanometer-sized magnesium oxide (MgO) powders investigated by an orthogonal test was that,the urea and amylum as the precipitator and the dispersant separate-ly,and the dosage of amylum was 45% on the condition of ultrasonic vibration 20 minutes at 70℃,and then by the process of the depositi-on,centrifugation,washing,solvent replacement,vacuum drying at room temperature and ultimately calcining. The results indicated that the dispersity of the nanoparticles was well, The crystal size was 12.5nm,they were well-proportioned,the crystallinity was high,and the productive rate reached 86%.This method will have a wide application.
A the preparation of nano-MgO via microemulsion method could realize the control of the particle size and the morphology,so micro- emulsion method has become an effective method to obtain nano-MgO, but there were not plenty of Researches dealing with the microemulsion method.reverse micelles were used as microreactors,so reagents disso-lving in the water shell reacted within the shell,and the influences of mass ratio of water to surfactant(w0) on UV-shielding properties of nano-MgO, assembly time,and calcination temperature on the particle size and morp-hologies of product were studied, the structure of the particles were characterized and the formation mechanism was discussed.
MgO nanoparticles have been prepared by polyethylene glycol octylphenyl ether(Triton X-100)/n-butyl alcohol/n-heptane/water reverse microemulsion.The result of thermal analysis (TG-DTG-DTA) of the precursor products showed that the proper calcination temperature was 600℃.The structures and morphologies of MgO nanoparticles were char-acterized by X-ray powder diffraction(XRD),Scanning electron micro-scope(SEM) and UV-vis spectrophotometry.The influences of mass ratio of water to surfactant(w0) on UV-shielding properties of nano-MgO, assembly time,and calcination temperature on the particle size and morp-hologies of product were studied,and the formation mechanisms in the reverse microemulsion were also discussed.The results show that the obtained MgO powder has no obvious agglomeration and narrow particle size distribution under the condition of mass ratio of water to surfactant wo= 15,calcination temperature r=600℃, assembly time of 15 h, reaction temperature t=30℃.
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。
Nano-MgO is a new type of high function fine inorganic material. Because of its quantum size effect, small-size effect, surface effect, macroscopic quantum tunneling effect, etc, it has a superior performance to the materials now existing.This paper introduced the current research status on nano-MgO,the theory of homogenous precipitation and micro-emulsion reaction.The nano-MgO crystal was made by the sluggish precipitation method from dolomite and reverse microemulsion method
In this paper,the dolomite which was native to Dongan Countr y, Yongzhou City of Hunan Province was used to make the nano-MgO by the homogenous precipitation method.And the orthogonal test methodused was used to find the optimum conditions under which the nana-MgO of small size and good dispersion could be obtained.The atomic absorption (AAS), X-ray diffraction (XRD),scanning electron microscopy (SEM) and thermogravimetric (TGA) were used to research the effect of dispersant types, dispersant dosage, precipitant types and solvent on the size of nano-MgO. A discussion was devoted to the mechanism of the impact of every factor with correlate theory. And the research could be usefull for the industrialization of nano-MgO.
The optimum technological conditions which was decided by the orthogonal test was:The optimum synthesis condition of nanometer-sized magnesium oxide (MgO) powders investigated by an orthogonal test was that,the urea and amylum as the precipitator and the dispersant separate-ly,and the dosage of amylum was 45% on the condition of ultrasonic vibration 20 minutes at 70℃,and then by the process of the depositi-on,centrifugation,washing,solvent replacement,vacuum drying at room temperature and ultimately calcining. The results indicated that the dispersity of the nanoparticles was well, The crystal size was 12.5nm,they were well-proportioned,the crystallinity was high,and the productive rate reached 86%.This method will have a wide application.
A the preparation of nano-MgO via microemulsion method could realize the control of the particle size and the morphology,so micro- emulsion method has become an effective method to obtain nano-MgO, but there were not plenty of Researches dealing with the microemulsion method.reverse micelles were used as microreactors,so reagents disso-lving in the water shell reacted within the shell,and the influences of mass ratio of water to surfactant(w0) on UV-shielding properties of nano-MgO, assembly time,and calcination temperature on the particle size and morp-hologies of product were studied, the structure of the particles were characterized and the formation mechanism was discussed.
MgO nanoparticles have been prepared by polyethylene glycol octylphenyl ether(Triton X-100)/n-butyl alcohol/n-heptane/water reverse microemulsion.The result of thermal analysis (TG-DTG-DTA) of the precursor products showed that the proper calcination temperature was 600℃.The structures and morphologies of MgO nanoparticles were char-acterized by X-ray powder diffraction(XRD),Scanning electron micro-scope(SEM) and UV-vis spectrophotometry.The influences of mass ratio of water to surfactant(w0) on UV-shielding properties of nano-MgO, assembly time,and calcination temperature on the particle size and morp-hologies of product were studied,and the formation mechanisms in the reverse microemulsion were also discussed.The results show that the obtained MgO powder has no obvious agglomeration and narrow particle size distribution under the condition of mass ratio of water to surfactant wo= 15,calcination temperature r=600℃, assembly time of 15 h, reaction temperature t=30℃.
引文
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