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Microwave-assisted preparation of coal-based heterogeneous acid catalyst and its catalytic performance in esterification

机译:微波辅助制备煤基多相酸催化剂及其酯化催化性能

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Powder coal is carbonized under nitrogen atmosphere and then treated with concentrate sulfuric acid with the assistance of microwave radiation for heterogeneous acid catalyst synthesis and the capability in catalyzing esterification of oleic acid with methanol for biodiesel production is subsequently studied. The catalysts are characterized by N-2 adsorption-desorption, ultimate analysis, X-ray diffraction, Raman spectra, attenuated total reflectance-Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and acid amount tests to obtain the physicochemical property. Microwave irradiation is a faster and simpler process than the conventional heating, and the sulfonation duration can be shortened to be 5 min. Under the carbonization temperature of 250 degrees C for 30 min and sulfonation temperature of 75 degrees C for 5 min, the synthesized catalyst gains the acid amount of 1.73 mmol g(-1) and esterification efficiency of 98.1% is achieved with the catalyst dosage mass percentage of 10 wt%, molar ratio of methanol to oleic acid of 12, esterification temperature of 65 degrees C and esterification duration of 180 min, where the commercial Amberlyst-15 catalyst only presents the efficiency of 71.5% under the same condition. Though the catalytic capability is crippled during the recycling reusage, it can be easily regenerated with its mostly original catalytic activity. (C) 2018 Elsevier Ltd. All rights reserved.
机译:粉煤在氮气氛下碳化,然后在微波辐射的帮助下用浓硫酸处理以合成多相酸催化剂,随后研究了催化油酸与甲醇的酯化反应以生产生物柴油的能力。通过N-2吸附-解吸,最终分析,X射线衍射,拉曼光谱,衰减全反射-傅里叶变换红外光谱,X射线光电子能谱和酸量测试来表征催化剂的理化性质。微波辐射是比常规加热更快,更简单的过程,磺化时间可缩短为5分钟。在炭化温度为250℃30分钟,磺化温度为75℃5分钟的条件下,合成的催化剂酸量为1.73 mmol g(-1),酯化效率为98.1%。在相同条件下,市售的Amberlyst-15催化剂的效率仅为10%(重量百分比),甲醇与油酸的摩尔比为12,酯化温度为65摄氏度,酯化持续时间为180分钟,而效率仅为71.5%。尽管在循环使用过程中,催化能力受到了损害,但可以通过其原始的催化活性轻松进行再生。 (C)2018 Elsevier Ltd.保留所有权利。

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