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首页> 外文期刊>New Journal of Chemistry >A high-surface-area mesoporous sulfated nano-titania solid superacid catalyst with exposed (101) facets for esterification: facile preparation and catalytic performance
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A high-surface-area mesoporous sulfated nano-titania solid superacid catalyst with exposed (101) facets for esterification: facile preparation and catalytic performance

机译：具有暴露的（101）小平面用于酯化的高表面积中孔硫酸盐化纳米二氧化钛固体超酸催化剂：简便的制备和催化性能

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摘要

In this paper, a high-surface-area mesoporous sulfated nano-titania exposed with (101) facets was prepared by a simple hydrothermai method without any template followed by surface sulfate modification. The physicochemical properties of the as-prepared catalyst were well characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), scanning electron microscopy (SEM), Raman spectroscopy (Raman), Fourier transform infrared spectroscopy (FTIR), N2 adsorption-desorption isotherms, temperature programmed desorption of NH3 (NH3-TPD), X-ray photoelectron spectroscopy (XPS) and pyridine adsorption infrared spectroscopy. The BET surface area of sulfated nano-titania with exposed (101) facets was 121 m~2 g~(-1). Well dispersed bidentate sulfate groups were linked 'to the exposed (101) facets of anatase nano-titania. Acid sites with moderate- and superacidic-strength formed in the sulfated titania catalyst. Also, the as-prepared sulfated sample possessed both Lewis and Brensted acid sites. The catalytic activity of sulfated nano-titania with exposed (101) facets was evaluated using the esterification reaction between acetic acid and n-butanol. It was found that the yield of butyl acetate increased to about 92.2% in the presence of the catalyst. Compared with the exposed (001) facets, the exposed (101) facets showed better catalytic activity of sulfated TiO2 in esterification. The effects of different reaction conditions were discussed in detail. Additionally, the as-prepared sulfated sample could be efficiently recycled and regenerated by simple soaking in sulfuric acid followed by calcination.
机译：本文采用无模板的简单水热法制备了具有（101）面的高表面积介孔硫酸盐纳米二氧化钛，并对其进行了表面硫酸盐修饰。制备的催化剂的理化性质通过X射线衍射（XRD），透射电子显微镜（TEM），高分辨率透射电子显微镜（HRTEM），扫描电子显微镜（SEM），拉曼光谱（Raman），傅里叶变换红外光谱（FTIR），N2吸附-脱附等温线，NH3的程序升温脱附（NH3-TPD），X射线光电子能谱（XPS）和吡啶吸附红外光谱。暴露的（101）小面的硫酸化纳米二氧化钛的BET表面积为121 m〜2 g〜（-1）。分散良好的二齿硫酸盐基团与锐钛矿型纳米二氧化钛的暴露面（101个）相连。在硫酸化二氧化钛催化剂中形成具有中等强度和超酸性强度的酸位。同样，所制备的硫酸化样品同时具有路易斯酸和布朗斯台德酸位。使用乙酸和正丁醇之间的酯化反应评估了具有暴露的（101）面的硫酸化纳米二氧化钛的催化活性。发现在催化剂存在下乙酸丁酯的产率增加到约92.2％。与暴露的（001）面相比，暴露的（101）面在酯化反应中表现出更好的硫酸化TiO2催化活性。详细讨论了不同反应条件的影响。另外，通过简单地浸泡在硫酸中然后煅烧，可以将如此制备的硫酸化样品有效地再循环和再生。

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