| 刘建平,杨小敏,王淑怡,吴丽丽,胡林.化学通报,2014,77(12):1224-1228. |
| 丝瓜络炭磺酸的制备及其催化合成糠醛 |
| Preparation of char sulfonic acid catalyst from Luffa Cylindrica for the synthesis of furfural |
| 投稿时间：2014-01-13 修订日期：2014-05-08 |
| DOI： |
| 中文关键词: 丝瓜络 炭磺酸 木糠 糠醛 |
| 英文关键词:Luffa Cylindrica char sulfonic acid xylose furfural |
| 基金项目: |
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| 中文摘要: |
| 以丝瓜络为炭源，浓硫酸为磺酸化试剂，制备了丝瓜络炭磺酸催化剂。利用中和滴定、X射线衍射仪（XRD）、傅立叶变换红外光谱仪（FT－IR）和热重－差热分析仪（TG－DTA）等手段对催化剂进行了表征。以表面酸密度为考察指标，确定了在300℃炭化3h，在80℃下磺化3h为最优的催化剂制备条件，此条件下丝瓜络炭磺酸催化剂表面酸密度可达1.119mmol/g。以木糠水解制备糠醛为探针反应，通过正交实验法考察了催化剂的实际催化活性。结果表明：在水解反应时间2h，水解反应温度200℃，催化剂用量占原料质量10%时，糠醛的平均收率达到78.69%，此时催化剂的催化活性最高。催化剂经第一次循环使用后性能有所下降，但随后的循环使用，催化性能稳定。将使用过的催化剂经再磺化，可基本恢复到新制催化剂的催化活性。 |
| 英文摘要: |
| A char sulfonic acid catalyst was prepared by using Luffa Cylindrica as raw materials and subsequent sulfonation. The catalysts were characterized by neutralization titration, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and thermogravimetric - differential thermal analyzer (TG-DTA). The preparation parameters on the catalyst activity was investigated using the acid density as the observed indexes .The results showed that the Luffa Cylindrica char sulfonic acid prepared under the optimal conditions of carbonization at 300 ℃ for 3 h and then sulphonation at 80℃ for 3 h exhibited highest catalytic activity, the acid density of the catalyst can reach 1.119mmol/g. The hydrolysis of xylose to furfural was taken as the model reaction to investigate the operational activity of the catalyst activity using orthogonal experiment design. The results showed that the catalysts have highest activities when using 10 wt % catalyst at 200℃ for 2h. The furfural yield could reach up to 78.69%. The catalyst performance drops after the first run but be stable for further use. The activities of the used catalysts can be fully restored if they were re-sulfonated. |
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