中孔金属氧化物（氧化铝、氧化镍等）的合成、表征及催化研究
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摘要
自1992年，M41S系列中孔氧化硅基材料的问世以来，不同化学组成的中孔材料作为一种新型材料引起了众多研究者的关注。而随着我国社会和经济的发展，石油资源结构和化工原料结构向重碳、大分子方向发展，要求使用具有大孔容、大表面积的催化剂来消除因原料结构大分子化带来的影响。作为使用最为广泛的催化剂和载体，制备具有大比表面积的中孔氧化铝材料具有极其重要的应用价值。在本论文中，采用两种不同的合成路线合成出了中孔氧化铝，并采用XRD、TG-DTA、TEM、SEM、N_2吸附、FTIR等表征手段对所合成的中孔氧化铝材料及其晶化过程和合成规律进行了考察。
以阴离子表面活性剂十二烷基磺酸钠(SDS)作为模板剂，我们首次得到了表面活性剂复合的氧化铝纳米管，直径在6-8nm，长度达到200nm以上。纳米管焙烧后就得到了中孔氧化铝AMA(Anionic，Mesoporous，Alumina)样品，500℃焙烧后AMA样品的比表面积为287.0m~2·g~(-1)，孔容为0.44cm~3·g~(-1)。
以中性的嵌段共聚物为模板剂，我们首次采用异丙醇铝为铝源替代常用的仲丁氧基铝制备了具有高热稳定性的中孔氧化铝NMA(Neutral，Mesoporous，Alumina)样品，在800℃焙烧后NMA样品仍保持了208.2m~2·g~(-1)的比表面积，孔容为0.44cm~3·g~(-1)。
在此基础上，制备了中孔Al_2O_3-NiO复合氧化物及中孔氧化铝为载体的Ni的催化剂，并采用XRF、TPR、H_2-TPD和H_2脉冲化学吸附等手段对催化剂进行了表征，并以1，2-二氯丙烷加氢脱氯制丙烯的反应对催化剂的催化性能进行了评价。中孔Al_2O_3-NiO复合氧化物中可以含有更高的Ni的含量，由此而具有了更好的活性和选择性。经过30h实验后，转化率仍保持在94％以上，丙烯的选择性保持在70％左右。
我们还以SDS为模板剂，对其他的过渡金属进行了中孔氧化物合成的尝试，得到了一种表面活性剂复合氧化铜的微米级管状结构，并对其形成的规律进行了考察，对其形成的机理进行了初步的讨论。
Since the successful synthesis of M41S mesoporous silica materials in 1992, considerable efforts have been directed towards the preparation of mesoporous materials with different chemical compositions. Along with the social and economic developments of our country, the energy-structure and raw materials of chemical industry develop towards heavy carbon and larger molecule, which request to use catalysts with larger surface areas and pore volumes to overcome the negative influence caused by the changes of raw materials structure. As the mostly used supports and catalysts, the synthesis of mesoporous alumina with large surface areas possesses huge values of economy and applications. In the present work, mesoporous alumina has been successfully prepared through two synthesis routes. The structures and properties of these materials have been studied by various techniques such as XRD, TG-DTA, TEM, SEM, physical adsorption and FTIR.
The alumina nanotubes have been prepared by using the anionic surfactant, sodium dodecyl sulfonate (SDS), as structure-directing template for the first time via a hydrothermal method. The obtained nanotubes are found having outer diameters from 6 to 8 nm with length up to 200 nm. After calcined at 500℃, the AMA (anionic, mesoporous, alumina) samples are obtained, with surface area of 287.0 m2·g~(-1) and pore volume of 0.44 cm3·g~(-1).
On the other hand, NMA (neutral, mesoporous, alumina) samples have also
以阴离子表面活性剂十二烷基磺酸钠(SDS)作为模板剂，我们首次得到了表面活性剂复合的氧化铝纳米管，直径在6-8nm，长度达到200nm以上。纳米管焙烧后就得到了中孔氧化铝AMA(Anionic，Mesoporous，Alumina)样品，500℃焙烧后AMA样品的比表面积为287.0m~2·g~(-1)，孔容为0.44cm~3·g~(-1)。
以中性的嵌段共聚物为模板剂，我们首次采用异丙醇铝为铝源替代常用的仲丁氧基铝制备了具有高热稳定性的中孔氧化铝NMA(Neutral，Mesoporous，Alumina)样品，在800℃焙烧后NMA样品仍保持了208.2m~2·g~(-1)的比表面积，孔容为0.44cm~3·g~(-1)。
在此基础上，制备了中孔Al_2O_3-NiO复合氧化物及中孔氧化铝为载体的Ni的催化剂，并采用XRF、TPR、H_2-TPD和H_2脉冲化学吸附等手段对催化剂进行了表征，并以1，2-二氯丙烷加氢脱氯制丙烯的反应对催化剂的催化性能进行了评价。中孔Al_2O_3-NiO复合氧化物中可以含有更高的Ni的含量，由此而具有了更好的活性和选择性。经过30h实验后，转化率仍保持在94％以上，丙烯的选择性保持在70％左右。
我们还以SDS为模板剂，对其他的过渡金属进行了中孔氧化物合成的尝试，得到了一种表面活性剂复合氧化铜的微米级管状结构，并对其形成的规律进行了考察，对其形成的机理进行了初步的讨论。
Since the successful synthesis of M41S mesoporous silica materials in 1992, considerable efforts have been directed towards the preparation of mesoporous materials with different chemical compositions. Along with the social and economic developments of our country, the energy-structure and raw materials of chemical industry develop towards heavy carbon and larger molecule, which request to use catalysts with larger surface areas and pore volumes to overcome the negative influence caused by the changes of raw materials structure. As the mostly used supports and catalysts, the synthesis of mesoporous alumina with large surface areas possesses huge values of economy and applications. In the present work, mesoporous alumina has been successfully prepared through two synthesis routes. The structures and properties of these materials have been studied by various techniques such as XRD, TG-DTA, TEM, SEM, physical adsorption and FTIR.
The alumina nanotubes have been prepared by using the anionic surfactant, sodium dodecyl sulfonate (SDS), as structure-directing template for the first time via a hydrothermal method. The obtained nanotubes are found having outer diameters from 6 to 8 nm with length up to 200 nm. After calcined at 500℃, the AMA (anionic, mesoporous, alumina) samples are obtained, with surface area of 287.0 m2·g~(-1) and pore volume of 0.44 cm3·g~(-1).
On the other hand, NMA (neutral, mesoporous, alumina) samples have also
引文
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