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模板法合成介孔氧化铝及其性能研究

Synthesis and Properties of Mesoporous Alumina with Template Method

【作者】 张豪杰

【导师】 王晶;

【作者基本信息】 大连交通大学 , 材料学, 2005, 硕士

【摘要】 本文分别以PEO-PPO-PEO三嵌段共聚物P123、月桂酸及月桂酸钠为模板剂,异丙醇铝为铝源,采用水热合成法得到了介孔结构的氧化铝。用TG、SEM、TEM、XRD、IR和N2吸附-脱附对样品进行了表征,来考察合成过程中pH值、水热合成时间、晶化温度、煅烧条件等对合成产物的组织、形貌和孔结构性能等的影响。 实验发现通过调节P123的用量,得到了孔道结构呈蠕虫状、比表面积在300m2/g左右、平均孔径在15nm左右、孔容在1.0cm3/g以上的氧化铝介孔材料;但其孔径分布稍宽,集中分布在5-30nm之间。实验结果证明,适当量的模板剂能够明显改善氧化铝介孔材料的孔结构特征。 与以P123作模板剂相比,通过采用月桂酸及月桂酸钠为模板剂合成出的介孔氧化铝在结构性能上表现出以下不同:合成的介孔氧化铝孔道颗粒更均匀,孔道排列规则、致密;孔径、孔容大幅度减小,平均孔径在6-7nm、孔容则减小到0.6m3/g:孔径分布明显变窄分布范围在2-11nm:比表面积有一定程度的增大,普遍达到400m2/g。 SEM、TEM、XRD等检测分析显示:经600℃煅烧所得产物为γ-Al2O3;进高压釜的样品介孔晶形更好,介孔排布更规整、紧密;煅烧后介孔具有短程有序、长程无序的特点。

【Abstract】 In this paper,by respectively using PEO-PPO-PEO block copolymer, C11H23COOH and C11H23COONa as template, using aluminum iso-propoxide as precipitator, the meso-structured alumina were synthesized under the method of hydro-thermal.TG,SEM,TEM,IR,XRD and N2 absorption-desorption were carried out to characterize the as-synthesized materials ,in order to investigate the factors affecting organization,morphology and porous structure of as-synthesized materials of synthesis procedure such as pH values、 time of hydrothermal synthesis、 crystallization temperature ,calcinations condition and so on.We can say from the experiments that by tuning the amount of P123, we achieved mesoporous alumina with worm-like porous 、 high surface area、 average pore sizes about 15nm、 pore volume over 1.0cm3/g,.But its have a slightly wide pore distribution which mostly concentrate on the scale of 5-30nm.The results show that proper amount of template can improve the pore properties of alumina obviously.Compared with using P123 as template ,the obtained samples with C11H23COOH and C11H23COONa as template show the following differences in structure properties.The particles become more homogenous and the porous structure become more regular.The pore diameter and volume reduce in a large extent.Their average pore size are at 6-7nm meanwhile the pore volume reduce to 0.6m3/g The pore distribution become narrow apparently by the rage of 2-11nm.The specific surface area increase in a certain extent and generally reach the value of 400m2/g.The analyst of SEM,TEM,XRD show that samples after calcinations at 600°C are γ-alumina. The samples crystal well when synthesized in autoclave. The pore structure become more normalized and compact.

  • 【分类号】TB383.4
  • 【被引频次】1
  • 【下载频次】609
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