| 冷冻方式对醛交联大豆蛋白多孔材料结构及吸附特性的影响 |
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| 引用本文： | 毕斌斌,林巧佳,郑培涛,李枫,欧阳庭,陈奶荣.冷冻方式对醛交联大豆蛋白多孔材料结构及吸附特性的影响[J].农业工程学报,2016,32(7):309-314. |
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| 作者姓名： | 毕斌斌 林巧佳 郑培涛 李枫 欧阳庭 陈奶荣 |
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| 作者单位： | 福建农林大学材料工程学院,福州,350002 |
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| 基金项目： | 国家自然科学基金资助项目（31470589，31500477）；福建省财政专项资金资助项目（K81600001）；福建农林大学重点建设项目专项（6112C0700001）；福建省教育厅科技计划项目（JA15185）。 |
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| 摘 要： | 为制备纳米级孔径的大豆蛋白多孔材料,研究了冰箱和液氮冷冻处理的醛交联大豆蛋白多孔材料的结构及吸附性能。结果表明:戊二醛对大豆蛋白的交联效果优于甲醛和乙二醛。液氮冷冻处理的多孔材料比表面积和孔容均较大,而平均孔径较小;纳米级孔的孔径都分布在80 nm以内,介孔总孔容占比超过50%,大孔次之,微孔占比最小;冰箱冷冻样品纳米级孔的孔径主要分布在70 nm以内,且微孔和介孔孔容都小于采用液氮冷冻处理的样品。场发射扫描电镜分析表明,大豆蛋白多孔材料的孔形态为微米级圆孔和纳米级狭缝孔。冷冻处理比醛类交联剂对孔结构的影响大,合适的冷冻方式能替代或超过交联剂种类变化取得的效果。热重分析表明液氮冷冻处理的戊二醛交联大豆蛋白多孔材料热稳定性好;该多孔材料对对硝基苯酚和六价铬离子具有一定的吸附效果,是制备大豆蛋白多孔材料较合适的方法。研究结果为植物蛋白多孔材料的制备提供参考。
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| 关 键 词： | 多孔材料 冷冻 吸附 大豆蛋白 醛 |
| 收稿时间： | 2015/11/8 0:00:00 |
| 修稿时间： | 2016/2/15 0:00:00 |
Effect of freezing treatment on structure and adsorption characteristic of soy protein porous materials crosslinked by aldehydes |
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| Bi Binbin,Lin Qiaoji,Zheng Peitao,Li Feng,Ouyang Ting and Chen Nairong.Effect of freezing treatment on structure and adsorption characteristic of soy protein porous materials crosslinked by aldehydes[J].Transactions of the Chinese Society of Agricultural Engineering,2016,32(7):309-314. |
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| Authors: | Bi Binbin Lin Qiaoji Zheng Peitao Li Feng Ouyang Ting and Chen Nairong |
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| Institution: | College of Material Engineering, Fujian Agriculture and Forestry University, Fuzhou 350002, China,College of Material Engineering, Fujian Agriculture and Forestry University, Fuzhou 350002, China,College of Material Engineering, Fujian Agriculture and Forestry University, Fuzhou 350002, China,College of Material Engineering, Fujian Agriculture and Forestry University, Fuzhou 350002, China,College of Material Engineering, Fujian Agriculture and Forestry University, Fuzhou 350002, China and College of Material Engineering, Fujian Agriculture and Forestry University, Fuzhou 350002, China |
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| Abstract: | The main goal of this work was to prepare porous materials using renewable soy protein as raw material. Soy protein was first blended with sodium hydroxide solution and crosslinked by aldehydes (formaldehyde, glyoxal and glutaraldehyde) to fabricate soy protein gel. The gel was then treated by freezing in refrigerator and liquid nitrogen to obtain porous materials after dry vacuum. A series of dynamic rheological tests were conducted for the gel, which included the strain sweep ranging from 0.5% to 120% at 1 Hz and the frequency sweep ranging from 0.13 to 3.6 Hz at 2% strain.Pore properties of these porous materials including the BET specific surface area, average pore diameter, pore size distribution and pore volume were characterized by the DFT method based on the nitrogen adsorption/desorption isothermal.The microstructure of porous materials was investigated by the field emission scanning electron microscope (FESEM). The thermostability of porous materials from ambient temperature to 600℃ in nitrogenwas investigated at the heating rate of 10℃/min by thermo gravimetric analysis technology. The results showed that the aldehydes crosslinked soy protein was efficient in forming gel. The storage modulus and loss modulus of soy protein gels were all increased as the scanning frequency increased, and the storage modulus was always higher than the loss modulus; the glutaraldehyde crosslinked soy protein gel had the highest storage modulus, as evidenced by rheological behavior analysis. These indicated that glutaraldehyde crosslinked protein was better than formaldehyde or glyoxal. Pore properties analysis results showed that aldehydes treatment porous materials had a higher BET specific surface area, a larger pore volume, and a smaller porous size than the control sample. Compared with the sample treated in refrigerator, the similar tendency was also observed on the porous materials treated by liquid nitrogen, which was that the diameter of nanoscale pore size was lower than 80 nm, the pore volume of mesoporous accounted for at least 50% of total pore volume, and the pore volume percentage decreased with the order of mesoporpus > macropore > micropore. All the refrigerator-treated porous materials showed the diameter of nanoscale pore size was lower than 70 nm. The BET specific surface area and pore volume of porous materials treated by liquid nitrogen had the decreased tendency with the order of glutaraldehyde > glyoxal > formaldehyde, indicating glutaraldehyde could be the crosslinking agent for soy protein porous material, but the freezing treatment had a greater influence on the pore structure than aldehydes did. This also could be evidenced by the nitrogen adsorption/desorption isothermal. The FESEM observations suggested that the pore patterns of all soy protein porous materials were micron grade circular pore and nanoscale slit pore, but the liquid nitrogen treatment resulted in more circular pore than the refrigerator treatment. Two times the mass loss (before 100℃ and after 200℃) occurred during the heating process of all samples, but soy protein porous material prepared from glutaraldehyde and liquid nitrogen treated soy protein showed better thermal stability after 440℃, indicating a better thermostability as evidenced by the thermo gravimetric analysis. There were 14.5%p-nitrophenol and 5.6% hexavalent chromium absorbed when glutaraldehyde and liquid nitrogen treated soy protein porous materials were soaked into the solution ofp-nitrophenol and potassium dichromate for 3 h, respectively. Therefore, glutaraldehyde and liquid nitrogen treated soy protein porous materials could be potentially applied as adsorption or thermal insulation materials, or prepare other porous materials such as carbon aerogel. |
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| Keywords: | porous materials freezing absorption soy protein aldehydes |
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