竹炭基固体磺酸催化剂的制备及其催化合成癸二酸二丁酯性能研究 |
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引用本文: | 饶兰,杨琴,蒋文伟. 竹炭基固体磺酸催化剂的制备及其催化合成癸二酸二丁酯性能研究[J]. 石油炼制与化工, 2014, 45(5): 66-71 |
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作者姓名: | 饶兰 杨琴 蒋文伟 |
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作者单位: | 1. 四川大学化工学院 2. 成都惠恩精细化工有限责任公司 |
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摘 要: | 以竹材为原料、氯磺酸为磺化剂,通过炭化-磺化法制备竹炭基固体磺酸催化剂,采用傅立叶红外光谱(FT-IR)、X射线衍射(XRD)、扫描电子显微镜仪(SEM)及热失重分析(TGA)等手段对催化剂进行表征,并将其用于催化癸二酸与正丁醇的酯化反应,考察制备条件对催化剂活性的影响。结果表明:竹炭基固体磺酸催化剂具有无定形炭结构,其热稳定性良好;合成催化剂的最佳条件为炭化温度325 ℃、炭化时间1 h、氯磺酸与竹炭配比2.5 mL/g、室温下磺化2 h,在此条件下制得的催化剂含酸量可达到1.77 mmol/g;在正丁醇与癸二酸摩尔比为3.0、反应时间为100 min、竹炭基固体磺酸催化剂用量为癸二酸质量的2.0 %、环己烷用量为3 mL的条件下,癸二酸转化率达99.14 %,重复使用4次后,癸二酸转化率仍可保持在80 %以上,说明催化剂性能稳定,具有良好的循环使用性能。
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关 键 词: | 竹炭 炭基固体磺酸催化剂 癸二酸 正丁醇 酯化反应 |
收稿时间: | 2013-10-21 |
修稿时间: | 2013-11-26 |
PREPARATION AND PERFORMANCE OF SULFONATED CHARCOAL-BASED SOLID ACID CATALYST FOR SYNTHESIS OF DIBUTYL SEBACATE |
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Abstract: | A novel charcoal-based sulfonated solid acid was synthesized through carbonation and then sulfonation of the bamboo charcoal using chlorosulfonic acid. The esterification of sebacic acid and n-butyl alcohol was taken as the model reaction to investigate the impact of preparation parameters on the catalyst activity. Fourier transform infrared spectroscopy(FT-IR)、X-ray diffraction(XRD)、scanning electron microscope(SEM)and thermo gravimetric analysis(TGA)were used to characterize the catalyst. The results show that the charcoal-based solid acid catalyst has amorphous carbon structure and the catalyst prepared at the optimal conditions of carbonization at 325 ℃ for 1h and then sulfonation at room temperature for 2 h with acid-bamboo charcoal ratio of 2.5ml/g exhibits a higher catalytic activity. Its acid group can be reached 1.77 mmol/g. The conversion rate of sebacic acid reached 99.14 % at the following conditions: n-butyl alcohol to sebacic acid mole ratio 3.0, the amount of charcoal-based sulfonated solid acid for 2% of sebacic acid, 3 ml n-butyl alcohol, and reaction time 100min. After repeated use 4 times, sebacic acid conversion rate remains above 80%, indicating the good regeneration performance. |
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