Yang Yang, Xu Yanyan, Han Baozhai, Xu Benjing, Liu Xinmei, Yan Zifeng
State Key Laboratory for Heavy Oil Processing, Chemical Engineering College, China University of Petroleum, Qingdao 266580, China.
J Colloid Interface Sci. 2016 May 1;469:1-7. doi: 10.1016/j.jcis.2016.01.053. Epub 2016 Jan 25.
Mesoporous alumina with pseudo-boehmite phase was prepared by using the cation-anion double hydrolysis method from mixed aqueous solution of aluminum sulfate and sodium aluminate. The effect of synthetic conditions on the crystal structure and textual properties of pseudo-boehmite was investigated, such as synthetic temperature, pH value and the addition of sodium silicate. With the assistance of characterization techniques, such as X-ray diffraction (XRD), N2 adsorption-desorption isotherms (BET) and (27)Al magic-angle spinning nuclear magnetic resonance (MAS NMR), the relationship between textural properties of the mesoporous alumina samples and their synthetic conditions was discussed. The results displayed that an increase in synthesis temperature promoted the formation of higher crystalline pseudo-boehmite with the increase of its surface area and pore volume. Pure pseudo-boehmite phase could be obtained in the pH value range from 6.0 to 9.0, while bayerite phase occurred when the pH value was over 10.0. The introduction of sodium silicate could greatly improve the pore volume (1.20 cm(3)/g) and surface area (480.2 m(2)/g) of pseudo-boehmite. Interestingly, pure pseudo-boehmite phase was obtained at very high pH value without formation of bayerite phase when sodium silicate was initially added into the aluminum hydroxide colloid.
采用阳离子 - 阴离子双水解法,以硫酸铝和偏铝酸钠的混合水溶液为原料制备了具有拟薄水铝石相的介孔氧化铝。研究了合成条件对拟薄水铝石晶体结构和织构性质的影响,如合成温度、pH值和硅酸钠的添加量。借助X射线衍射(XRD)、N₂吸附 - 脱附等温线(BET)和²⁷Al魔角旋转核磁共振(MAS NMR)等表征技术,探讨了介孔氧化铝样品织构性质与其合成条件之间的关系。结果表明,合成温度升高促进了高结晶度拟薄水铝石的形成,其比表面积和孔体积增加。在pH值为6.0至9.0的范围内可获得纯拟薄水铝石相,而当pH值超过10.0时会出现拜耳石相。硅酸钠的引入可大大提高拟薄水铝石的孔体积(1.20 cm³/g)和比表面积(480.2 m²/g)。有趣的是,当将硅酸钠最初加入氢氧化铝胶体时,在非常高的pH值下可获得纯拟薄水铝石相,且不会形成拜耳石相。