白石墨烯泡沫的无模板大产量制备及其应用

发布时间：2018-06-22 07:40

  本文选题：白石墨烯泡沫 + 多孔氮化硼　； 参考：《南京航空航天大学》2015年硕士论文

【摘要】：多孔氮化硼除具有高稳定性、高导热、低摩擦和良好的透波性等属性外,还具有高比表面积和独特的孔径分布的特征,在催化剂载体、储能材料、高分子填料等领域具有广泛的应用前景。多孔氮化硼的制备是研究其性能和推广其应用的前提,目前多孔氮化硼的制备方法主要有水热合成法、模板法、先驱体热解法和气凝胶技术,但这些方法的合成工艺一般都比较繁琐而且产量较低,大大限制了多孔氮化硼材料的应用和发展。因此,寻求一种合适的、简单易行的方法来制备具有高质量、高产率、高比表面积的多孔氮化硼具有十分重要的意义。本文采用无模板的一步合成法制备出具有不同微观形貌的多孔氮化硼,研究其属性并针对其结构特征应用于催化剂载体、环境治理、高分子复合等领域。以硼烷氨为原料,硫脲、氨基硫脲为发泡剂,通过简单的高温热分解反应,即可制备出白色泡沫状的多孔氮化硼。产率可以达到68%、表观密度可以低至2.05 mg cm-3,比商业氮化硼的理论密度(2.27 g cm-3)低三个数量级,这种的超轻物质能站立在蒲公英上而没有压弯其晶须。当发泡剂为硫脲时,可以得到由不规则骨架支撑、大面积薄片连接的三维多孔氮化硼,产物标记为ABSN。HRTEM显示出ABSN产物的薄片结构上具有多孔结构,片层可以达到单层、双层、三层的原子厚度;氮气吸附脱附结果表明ABSN的比表面积为681 m2 g-1,平均孔径为1.5和32 nm。当发泡剂为氨基硫脲时,可以得到三支叉、四支叉相互连接的网络纤维状的多孔氮化硼,产物标记为ABSD。SEM显示出ABSD产物的纤维长度可以达到几百微米;氮气吸附脱附结果表明ABSN的比表面积为128 m2 g-1,平均孔径为15 nm。以聚乙二醇为反应溶液、硝酸银为原料、ABSN产物为催化剂载体,采用紫外光辐射的方法制备出Ag/ABSN催化剂。Ag/ABSN催化剂对甲醇不仅显示出良好的催化性能(T50、T95分别只有50 oC和110 oC,远低于Ag/γ-Al2O3催化剂对应的这两个数值110 oC、180 oC),而且在高温下能维持很好的稳定性。以ABSN产物为吸附剂,对有机溶剂、油进行吸附,吸附能力可以达到70-191 g g-1,吸附能在瞬间完成,且可以多次循环利用。对甲基蓝、甲基橙染料的吸附能在5 min之内完成80%以上的吸附,最大吸附能力将近500 mg g-1。以ABSD产物为添加剂,SD184为基体材料,采用热固成型工艺可以制备出不同ABSD含量的ABSD/SD 184复合材料。随着氮化硼纤维含量的增加,ABSD/SD 184复合材料的耐热性逐渐增加;1 wt%的复合材料在600 nm处具有83%的透光率;5 wt%的复合材料的机械强度为96MPa,弹性模量为3.46GPa;50 wt%的复合材料的热导率可以增加至114.7 W m-1 K-1。
[Abstract]:In addition to the properties of high stability, high thermal conductivity, low friction and good permeability, porous boron nitride also has the characteristics of high specific surface area and unique pore size distribution. Polymer fillers and other fields have a wide range of applications. The preparation of porous boron nitride is the premise of studying its properties and popularizing its application. At present, the main preparation methods of porous boron nitride are hydrothermal synthesis, template method, precursor pyrolysis and aerogel technology. However, the synthetic process of these methods is generally cumbersome and low yield, which greatly limits the application and development of porous boron nitride materials. Therefore, it is of great significance to find a suitable and simple method to prepare porous boron nitride with high quality, high yield and high specific surface area. In this paper, porous boron nitride with different micromorphology was prepared by one-step synthesis without template. The properties of boron nitride were studied and applied in the fields of catalyst carrier, environmental treatment, polymer compound and so on. Using borane ammonia as raw material thiourea and thiosemicarbazone as foaming agent the white foam porous boron nitride can be prepared by a simple high temperature thermal decomposition reaction. The yield can reach 68% and the apparent density can be as low as 2.05 mg / cm ~ (-3), which is three orders of magnitude lower than the theoretical density of commercial boron nitride (2.27 g cm-3). This ultra-light substance can stand on dandelion without bending its whisker. When the foaming agent is thiourea, three dimensional porous boron nitride supported by irregular skeleton and connected by large area thin sheet can be obtained. The product labeled ABSN. HRTEM shows that the sheet structure of ABSN product has porous structure, and the lamellar layer can reach single layer and double layer. The atomic thickness of the three layers and the nitrogen adsorption and desorption results show that the specific surface area of ABSN is 681 m ~ 2 g ~ (-1) and the average pore size is 1.5 and 32 nm. When the foaming agent is thiosemicarbazone, the porous boron nitride with three forks and four forks connected to each other can be obtained. The product labeled ABSD. SEM shows that the fiber length of ABSD product can reach several hundred microns. The results of nitrogen adsorption and desorption show that the specific surface area of ABSN is 128 m ~ 2 g ~ (-1) and the average pore size is 15 nm 路m ~ (-1). Using polyethylene glycol as reaction solution, silver nitrate as raw material, ABSN product as catalyst carrier, Ag/ ABSN catalyst. Ag- / ABSN catalyst showed good catalytic performance for methanol by ultraviolet radiation method (T50 T95 is only 50 OC and 110oC, which is much lower than that of Ag/ 纬 -Al _ 2O _ 3 catalyst (110oC ~ (180 OC), and at high temperature, the catalyst has good catalytic performance for methanol (T50 / ABSN catalyst is only 50 OC and 110oC), which is much lower than that of Ag/ 纬 -Al _ 2O _ 3 catalyst. Can maintain good stability. Using ABSN product as adsorbent, the adsorption ability of organic solvent and oil can reach 70-191 g g ~ (-1), the adsorption energy can be achieved in an instant, and can be reused many times. The adsorption of methyl blue and methyl orange dyestuffs can reach more than 80% in 5 min, and the maximum adsorption capacity is nearly 500mg g ~ (-1). ABSD / SD184 composites with different ABSD content can be prepared by thermosetting process using ABSD product as additive and SD184 as matrix material. With the increase of boron nitride fiber content, the heat resistance of ABSD / SD 184 composites increases gradually. The mechanical strength and elastic modulus of the composites with a transmittance of 83% or 5 wt% at 600 nm are 96 MPA and 3.46 GPA / 50 wt% respectively, and the mechanical strength of the composites is 96 MPA and the elastic modulus is 3.46 GPA / 50 WTT% at 600 nm. The thermal conductivity can be increased to 114.7 W m-1 K-1.
【学位授予单位】：南京航空航天大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ128.1

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