硝酸钾负载介孔炭催化光皮树油酯交换反应研究

doi:10.3969/j.issn.0253-2417.2021.06.011

摘要/Abstract

摘要：

以蔗糖为原料，SBA-15为模板剂，采用硬模板法制备介孔炭CMK-3，CMK-3负载KNO₃制得介孔炭基固体碱催化剂KNO₃/CMK-3，并将KNO₃/CMK-3用于催化光皮树油酯交换反应制备生物柴油。以生物柴油酯交换率为评价指标，通过单因素试验对固体碱催化剂KNO₃/CMK-3最佳制备条件进行探索，结果表明：在焙烧温度450 ℃、焙烧时间2 h、KNO₃负载量7.5%，制得的7.5% KNO₃/CMK-3催化性能最佳，催化光皮树油（20 g）合成生物柴油酯交换率可达95.95%。使用SEM、TEM、BET、XRD、CO₂-TPD等检测手段对催化剂进行表征，7.5% KNO₃/CMK-3的碱量0.921 1 mmol/g，比表面积93.95 m²/g，总孔容0.114 6 cm³/g，孔径4.879 nm，改性前后，介孔炭碱性活性分子负载其上，炭骨架棒状结构保持良好。FT-IR、GC-MS等分析表明：制得的生物柴油产品中亚油酸甲酯和油酸甲酯质量分数最高，分别为45.97%和32.08%。

关键词: 生物柴油, 光皮树油, 酯交换反应, 固体碱催化剂, CMK-3

Abstract:

Using sucrose as the carbon source and SBA-15 as the mesoporous template, the CMK-3 mesoporous carbon was prepared by the hard template method. And then, the mesoporous carbon-based solid base catalyst by loading KNO₃ that could efficiently catalyze the production of biodiesel from Cornus wilsoniana oil was prepared by the impregnation method. Catalytic experiments were carried out to determine the catalytic activity of KNO₃/CMK-3 and explore the best preparation conditions by comparing the transesterification rate of biodiesel. The catalyst was characterized by SEM, TEM, BET, XRD, CO₂-TPD, etc.. The research results showed that the optimal loading conditions were calcination temperature 450 ℃, calcination time 2 h, loading amount of KNO₃ 7.5%. Under these conditions, the transesterification rate of biodiesel from C.wilsoniana oil could reach 95.95%. The catalyst 7.5%KNO₃/CMK-3 was characterized by SEM, TEM, BET, XRD, CO₂-TPD and so on, the results showed that the alkali content of the catalyst 7.5%KNO₃/CMK-3 was 0.921 1 mmol/g, the surface area was 93.95 m²/g, the total pore volume was 0.114 6 cm³/g and the pore size was 4.879 nm. Before and after the modification, the alkaline active molecule was loaded on the meso-carbon and the rodstructure of carbon skeleton remained stable. The FT-IR and GC-MS analysis results showed that the mass fractions of methyl linolenate and methyl oleate in the obtained biodiesel were the highest, and were 45.97% and 32.08%.

Key words: biodiesel, Cornus wilsoniana oil, transesterification reaction, solid base catalyst, CMK-3

中图分类号:

TQ35

王钦, 汪红梅, 张爱华, 肖志红, 李昌珠. 硝酸钾负载介孔炭催化光皮树油酯交换反应研究[J]. 林产化学与工业, 2021, 41(6): 83-89.

Qin WANG, Hongmei WANG, Aihua ZHANG, Zhihong XIAO, Changzhu LI. KNO₃-Loaded Mesoporous Carbon Catalyzed Transesterification Reaction of Cornus wilsoniana Oil[J]. Chemistry and Industry of Forest Products, 2021, 41(6): 83-89.

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样品 sample	比表面积/(m²·g^-1) specific surface area	总孔容/(cm³·g^-1) total pore volume	孔径/nm pore size
CMK-3	500.25	0.4887	3.9075
7.5%KNO₃/CMK-3	93.95	0.1146	4.8790

峰号 No.	化合物名称 compound	相对峰面积% relative peak area
1	棕榈酸甲酯palmitic acid methylester	15.2466
2	棕榈油酸甲酯methyl palmitoleate	1.1679
3	硬脂酸甲酯methyl stearate	1.8278
4	油酸甲酯methyl oleate	32.0802
5	亚油酸甲酯methyl linolenate	45.9672
6	其他other	3.7102

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