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Preparation of a coal tar pitch-based solid acid catalyst and its esterification activity in ethyl acetate production

机译:煤焦油沥青基固体酸催化剂的制备及其在乙酸乙酯生产中的酯化活性

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In this work, carbon-based solid acid catalysts have been prepared by a series of treatments for coal tar pitch (CTP). The modified coal tar pitch (MCTP) modified with trichloroacetic acid was sulfonated by concentrated sulfuric acid. An orthogonal array design was used to optimize the preparation conditions. The catalyst from MCTP had a higher acid density than from CTP. It possessed an acid site density of 7.01 mmol g~(-1) under the optimum conditions (sulfonation temperature of 155 °C, reaction time of 12 h and sulfuric acid/MCTP mass ratio of 3:1). FT-IR spectroscopy was used for structural analysis. The elemental composition and acid site density for the solid acid were analyzed by elemental analyzer and volumetric titration, respectively. The catalytic ability of the solid acid was observed through the esterification reaction of ethyl acetate. The results showed that the yield of ethyl acetate with 86.67 wt% was obtained under the best conditions of the single factor tests (reaction time of 60 min, ethanol/ethanoic acid mass ratio of 3:1, catalyst dosage of 5 wt%). The catalysts retained satisfactory catalytic activity for esterification of ethyl acetate after five catalytic cycles.
机译:在这项工作中,通过对煤焦油沥青(CTP)进行了一系列处理,制备了碳基固体酸催化剂。用浓硫酸磺化用三氯乙酸改性的改性煤焦油沥青(MCTP)。正交阵列设计用于优化制备条件。来自MCTP的催化剂具有比来自CTP的催化剂更高的酸密度。在最佳条件下(磺化温度为155°C,反应时间为12 h,硫酸/ MCTP质量比为3:1),其酸位密度为7.01 mmol g〜(-1)。 FT-IR光谱用于结构分析。通过元素分析仪和体积滴定法分别分析了固体酸的元素组成和酸位密度。通过乙酸乙酯的酯化反应观察到固体酸的催化能力。结果表明,在单因素试验的最佳条件下(反应时间为60分钟,乙醇/乙酸质量比为3:1,催化剂用量为5 wt%),乙酸乙酯的收率为86.67 wt%。在五个催化循环后,该催化剂保留了令人满意的乙酸乙酯酯化催化活性。

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