木棉基炭气凝胶的制备、表征及其吸附性能研究

doi:10.3969/j.issn.0253-2417.2021.02.007

摘要/Abstract

摘要：

以木棉为原料，采用均质-常压干燥-炭化法制备出了中空管状的木棉基炭气凝胶（KFCA）。利用SEM、氮气吸附/脱附、XRD、拉曼光谱、FT-IR、XPS和接触角测试对KFCA的表面形貌、孔隙结构、晶相结构和表面化学组成进行表征，并以常见的有机溶剂及油类为吸附质研究了KFCA的吸附性能。研究结果表明：KFCA具有独特的中空管状结构，且表现出低密度、表面疏水、比表面积大和孔隙发达等优点。800℃炭化温度下制备的KFCA（KFCA-800）的水接触角为134.0°，比表面积为170.22 m²/g，平均孔径为4.022 nm，孔容积为0.22 cm³/g；KFCA-800由C、H、O组成，其中C主要以CO和CC官能团形式存在。炭化温度对KFCA吸附性能有一定的影响，其中以KFCA-800吸附性能最佳，对泵油、大豆油、二甲基甲酰胺（DMF）、乙醇、丙酮、正己烷、苯和二甲苯的吸附容量分别可达52.3、34.15、75.21、72.26、54.16、52.79、62.06和38.95 g/g。此外，KFCA可以通过简单的干燥和萃取-干燥法再生，KFCA-800在循环吸附5次后，对乙醇的吸附容量为69.54 g/g（达初始吸附量的90%以上），对大豆油的吸附容量为26.16 g/g（达到初始吸附量的75%左右）。

关键词: 木棉纤维, 炭气凝胶, 常压干燥, 中空管状, 吸附

Abstract:

A kapok fiber carbon aerogel(KFCA) with hollow tubular structure was synthesized through the homogenous treatment, ambient pressure drying and carbonization. The surface morphology, pore structure, crystal structure and chemical composition of KFCA were characterized by scanning electron microscopy(SEM), N₂ adsorption/desorption isotherms, X-ray diffraction (XRD), Raman spectroscopy, Fourier transform infrared(FT-IR) spectroscopy, X-ray photoelectron spectroscopy(XPS) and water contact angle(WCA). The adsorption properties of KFCA were studied with the commonly used organic reagents and oils as adsorbate. The results indicated that KFCA had an unique hollow tubular structure with low density, hydrophobic surface, large specific surface area and developed pores. The water contact angle of KFCA-800(which was carbonized at 800 ℃) was 134.0°, specific surface area was up to 170.22 m²/g, the average pore diameter was 4.022 nm and the pore volume was 0.22 cm³/g. KFCA-800 was composed of C, H and O. C=O and C=C functional groups were detected on the surface of KFCA-800. Carbonization temperature had a certain effect on the adsorption performance of KFCA, among which KFCA-800 had the best adsorption performance. Its adsorption capacities of pump oil, soybean oil, N, N-dimethylformamide(DMF), ethanol, acetone, n-hexane, benzene and xylene were reach up to 52.3, 34.15, 75.21, 72.26, 54.16, 52.79, 62.06 and 38.95 g/g. In addition, KFCA could be regenerated by the methods of direct drying and extraction-drying. The adsorption capacities of KFCA-800 for ethanol and soybean oil were 69.54 g/g (more than 90% of the initial adsorption capacity) and 26.16 g/g (about 75% of the initial adsorption capacity) respectively after five adsorption-regeneration cycles.

Key words: kapok fiber, carbon aerogel, ambient pressure drying, hollow tubular structure, adsorption

中图分类号:

TQ35

侯浩强, 孙文野, 李双宾, 苗祥森, 刘守新. 木棉基炭气凝胶的制备、表征及其吸附性能研究[J]. 林产化学与工业, 2021, 41(2): 47-54.

Haoqiang HOU, Wenye SUN, Shuangbin LI, Xiangsen MIAO, Shouxin LIU. Preparation, Characterization and Adsorption Properties of Kapok-based Carbon Aerogels[J]. Chemistry and Industry of Forest Products, 2021, 41(2): 47-54.

图/表 7

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样品samples	比表面积/(m²·g^-1)BET specific surface area	孔容积/(cm³·g^-1)total pore volume	平均孔径/nmaverage pore diameter
KFCA-600	51.35	0.09	8.598
KFCA-700	134.29	0.17	7.295
KFCA-800	170.22	0.22	4.022
KFCA-800^*	156.61	0.19	4.108
KFCA-900	192.48	0.32	3.286

样品samples	乙醇alcohol	丙酮acetone	正己烷n-hexane	苯benzene	二甲苯xylene	二甲基甲酰胺DMF	泵油pump oil	大豆油soybean oil
KFCA-600	66.42	37.12	47.00	57.36	39.04	71.11	45.72	26.16
KFCA-700	70.34	49.62	48.37	53.45	40.58	67.79	48.49	31.41
KFCA-800	72.26	54.16	52.79	62.06	38.95	75.21	52.30	34.15
KFCA-900	57.87	52.38	38.42	55.31	48.86	82.78	53.68	30.49

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