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Preparation, characterization, and application of ordered mesoporous S2O82-/ZrO2-SiO2 with high specific surface area

机译:具有高比表面积的有序介孔S2O82- / ZrO2-SiO2的制备,表征和应用

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摘要

A series of ordered mesoporous S2O82-/ZrO2-SiO2 (OMSZS) solid superacids with different calcination temperatures (400-650 degrees C) was synthesized using zirconium n-propoxide and tetraethyl orthosilicate as the raw materials and P123 as a structure-directing agent by solvent evaporation-post-dipping method. Transmission electron microscopy and small-angle X-ray diffraction results showed that the OMSZS were all ordered. The nitrogen adsorption results indicated that the specific surface area of OMSZS could reach up to 331-385 m(2)/g, whereas the average pore diameters were in the range of 3.1-3.2 nm. The pyridine infrared results mainly displayed Lewis acids, and the ammonia (NH3)-temperature programmed desorption characterization showed that the NH3 desorption of the OMSZS calcined at 550 degrees C was 61 cm(3)/g STP. The catalytic performance of the OMSZS was investigated by the transesterification reaction of waste frying oil and methanol. The yield of fatty acid methyl ester could reach up to 94% at 200 degrees C reaction temperature for 6 h. After repeated use for four times, the catalyst still featured good activity and the yield was 78%.
机译:使用锆N-丙醇氧化锆和作为原料和P123作为结构引导剂,合成具有不同煅烧温度(400-650摄氏度)的一系列有序的介孔S2O82- / ZrO2-SiO 2(OMSZ)固体超级酸(400-650℃)。溶剂蒸发后浸渍法。透射电子显微镜和小角度X射线衍射结果表明OMSZ全部有序。氮吸附结果表明OMSZ的比表面积可达331-385米(2)/ g,而平均孔径在3.1-3.2nm的范围内。吡啶红外结果主要展示路易斯酸,氨(NH3) - 温度编程的解吸表征显示,在550℃下煅烧的OMSZ的NH3解吸为61cm(3)/ g STP。通过废油炸油和甲醇的酯交换反应研究了OMSZ的催化性能。脂肪酸甲酯的产率可在200℃的反应温度下达到94%,6小时。重复使用四次后,催化剂仍然具有良好的活性,产率为78%。

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