大豆分离蛋白质和聚氨酯改性聚丙烯腈纤维的研究
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摘要
大豆蛋白质来源于轧油后的豆粕,可再生降解,与来自动物资源的蛋白质相比价格低廉。大豆蛋白质在材料领域应用研究有利于解决日益严重的环境问题,噌加农副产品的附加值。因此近年来,视为石油基高分子的替代物之一的大豆分离蛋白质(SPI),广泛应用于塑料、粘合剂、纺织材料等领域。
聚丙烯腈(PAN)和聚氨酯(PU)作为通用高分子材料,具有优良的性能。在材料加工中,通过共混可以综合多组分体系的优良性能,获得性能更加突出的新材料。添加适量尿素(Urea)的二甲亚砜(DMSO)可以溶解SPI,而二甲亚砜为聚丙烯腈、聚氨酯的良溶剂,因此本文首次研究了SPI在DMSO/Urea中的分散状态及其特性;PAN/SPI/PU多组分体系分子间的相互作用和相容增容情况;SPI在DMSO/Urea和PAN/SPI/PU多组分体系在DMSO中的流变特性;通过湿法纺丝制备PAN/SPI/PU共混纤维,表征分析了纤维纺丝成型机理及其结构性能。
考察了大豆分离蛋白在二甲亚砜/尿素中的溶解特性,实验结果显示SPI在所研究条件下最大溶解度约为4.8%。Urea是SPI能在DMSO中溶解的重要因素,而热处理条件影响SPI在DMSO中的溶解,在实验范围内,合适的尿素浓度、热处理温度和时间为分别3M,90℃,2h。随urea浓度增加,SPI在DMSO/Urea中凝胶化的临界浓度增大,当DMSO浓度达到一定值后,临界浓度随DMSO浓度增大变化不大。随SPI浓度不同,在DMSO/Urea中呈现溶液、溶胶、凝胶三种状态。
相容性是影响多组分高聚物体系结构性能的重要因素,本文通过红外光谱、混合热计算、稀溶液粘度法、玻璃化转变温度法及显微镜形态观察法对多组分体系分子间的相互作用和相容性进行表征分析。研究结果表明,SPI/PU具有部分相容性,而PAN/SPI、PAN/PU的相容性差,但仍然存在弱的分子间相互作用。PAN/SPI/PU体系有明显相分离现象,体系相容性差。合成制备了丙烯腈─大豆分离蛋白接枝共聚物(AN-g-SPI)和水解聚丙烯腈(HPAN)作为相容剂,随AN-g-SPI、HPAN含量增加共混膜的力学性能改善。
流变性能直接影响着纤维的纺丝成型过程和所制备纤维的结构性能。实验结果发现SPI在DMSO/Urea中剪切变稀,随浓度增加,由于其分散状态发生变化,则流动行为差异加大。原液浓度影响共混溶液的流动和成丝性,当含固量为23%时,纺丝原液的成丝性最好。SPI和PU对PAN流变性能的影响相反,SPI的加入降低了PAN溶液流动性,PAN/SPI溶液的非牛顿指数随SPI含量增加呈下降趋势,结构粘度指数则呈增加趋势。PAN/SPI/PU多组分体系的流变性能受SPI和PU含量的影响较大,可通过调整组分改变流动行为。SPI和PU的加入降低了PAN/DMSC溶液对温度的敏感性,升温有助于改善体系的流动性。
PAN/SPI/PU纤维成型机理的研究中主要探讨了凝固浴浓度和温度、拉伸比的分配比例和倍数、干燥致密化的温度和时间、交联剂的种类和浓度对其成型及性能的影响。实验结果表明:凝固浴浓度60%、温度22℃,预拉伸倍数1.5-2倍,纤维拉伸性能好。120℃干燥致密化15-20min可得强度高而干燥致密化时间也合适的纤维。采用在凝固浴中添加交联剂的方法以改善PAN/SPI纤维的性能。比较乙二醛和戊二醛的作用后,发现乙二醛加入可明显改善纤维拉伸性能,纤维拉伸强度提高近2倍,随乙二醛浓度提高纤维性能提高,但浓度超过10%后改善作用不明显。
利用红外光谱、蛋白酶水解法、表面接触角、回潮率、DSC、TGA、力学性能测试、酸性染料染色等方法对PAN/SPI/PU纤维结构性能分析表征显示:PAN/SPI/PU纤维中确实含有PAN、SPI和PU共同的特征吸收峰,然而在实验范围内蛋白酶水解法发现所测纤维中的蛋白质含量比理论添加量少。随SPI含量的增加,纤维热分解起始和峰值温度略向低温方向移动;具有部分生物降解性能;酸性染料染色性能提高;纤维的表面接触角减小,吸湿性提高。
Soy protein isolated (SPI) has been considered recently as an alternative to petroleum polymer in the manufacture of adhesives, plastics, textiles et al. Soy protein is available from renewable resources and biodegradable. Utilizing soy protein for materials will help to solve environmental and petroleum resource problems and add value for agricultural by-products.
Polyacrylonitrile (PAN) and polyurethane (PU) are general polymer material, and they have excellent performance, respectively. Blending is an important method in polymer manufacture, which may combine the advantages of both components. In this paper, the dispersion states and rheological properties of SPI in dimethylsulphoxide/urea, miscibility, interactions and rheological properties of PAN/SPI/PU system in DMSO, structure-property relationships of PAN/SPI/PU fiber were studied.
Dimethylsulfoxide(DMSO)/urea was chosen as a mixture solvent system to dissolve soy protein. The dispersion status and properties of SPI in DMSO/urea were studied. The result showed that SPI has relatively high solubility in DMSO/urea mixture solvent and urea served as a key factor of dissolving SPI in the system. The solubility properties and gelation phenomenon of SPI were studied in DMSO/Urea. The effects, such as heating time, temperature and concentration of urea were discussed. SPI in the DMSO/urea mixture system exhibited different dispersion statuses with increasing of SPI content.
Miscibility and interaction properties of PAN/SPI blend systems were studied by using methods of fourier transform infrared(FTIR), heat of mixing, dilute solution viscometry, phase contrast microscope. It was found that SPI/PU was partly miscilbility system and PAN/SPI, PAN/PU was immiscible system respectively, however there existed attractive interaction. In order to promote the compatibility, the main products of graft copolymerization of acrylonitrile and SPI (AN-g-SPI) and the alkaline hydrolysis polyacrylonitrile (HPAN) were used as the compatibilizers, and the mechanical properties of blends were improved observably.
The SPI dispersed system in DMSO/Urea was shear-thinning fluid and flow behavior was different with increasing content of SPI because the change of dispersed state. The effects of SPI and PU on the rheological properties of PAN solutions were opposite. The Non-Newtonian index of PAN/SPI solutions decreased and corresponding structure viscosity index of that increased with increasing of SPI content on the whole. The fluid properties of PAN solution was worsened with the addition of SPI. The rheological properties of PAN/SPI/PU solutions were affected by the contents of SPI and PU. In any case, the increase of temperature contributed to the improvement of the fluid properties of blend solutions.
The effect of temperature and concentration of coagulation bath, the multiple and corresponding distributive proportion of multiple drawing, temperature and time of drying, the type and concentration of crosslink agent on the properties of blend fiber were investigated. The result shown it was better to get good performance fibres when the concentration of coagulating agent was 60%, and the temperature of coagulation bath was 22℃, the drawing multiple in washing bath was 1.5-2 and the drying time was 15-20 minutes at 120℃.The effect of glutaraldehyde and glyoxal as cross-linking agent at coagulation bath on PAN/SPI fiber were studied. It was found that the mechanical properties of fibres used by glyoxal were improved.
The methods of fourier transform infrared(FTIR), enzymatic hydrolysis, scanning electron microscopy(SEM), differential scanning calorimetry (DSC), thermal gravimetric analysis (TGA), mechanical property, dye adsorption, contact angle and moisture regain measurements were employed to investigate the structure and properties of PAN/SPI/PU fiber. The results show that the concentration of SPI in PAN/SPI/PU fibers determinately increased with increasing of addition SPI by using enzymatic hydrolysis though there was loss of SPI content compared with addition of SPI weight. The PAN/SPI/PU fibers were partly biodegrability system. The thermo degraded temperature slightly decreased with increasing of content of SPI in the PAN/SPI fiber. The dye adsorption for acidic dye and moisture regain of PAN/SPI fibers increased and the contact angle of that decreased with increasing of SPI ratio as well as compared with a referenced PAN fiber prepared via the same method.
聚丙烯腈(PAN)和聚氨酯(PU)作为通用高分子材料,具有优良的性能。在材料加工中,通过共混可以综合多组分体系的优良性能,获得性能更加突出的新材料。添加适量尿素(Urea)的二甲亚砜(DMSO)可以溶解SPI,而二甲亚砜为聚丙烯腈、聚氨酯的良溶剂,因此本文首次研究了SPI在DMSO/Urea中的分散状态及其特性;PAN/SPI/PU多组分体系分子间的相互作用和相容增容情况;SPI在DMSO/Urea和PAN/SPI/PU多组分体系在DMSO中的流变特性;通过湿法纺丝制备PAN/SPI/PU共混纤维,表征分析了纤维纺丝成型机理及其结构性能。
考察了大豆分离蛋白在二甲亚砜/尿素中的溶解特性,实验结果显示SPI在所研究条件下最大溶解度约为4.8%。Urea是SPI能在DMSO中溶解的重要因素,而热处理条件影响SPI在DMSO中的溶解,在实验范围内,合适的尿素浓度、热处理温度和时间为分别3M,90℃,2h。随urea浓度增加,SPI在DMSO/Urea中凝胶化的临界浓度增大,当DMSO浓度达到一定值后,临界浓度随DMSO浓度增大变化不大。随SPI浓度不同,在DMSO/Urea中呈现溶液、溶胶、凝胶三种状态。
相容性是影响多组分高聚物体系结构性能的重要因素,本文通过红外光谱、混合热计算、稀溶液粘度法、玻璃化转变温度法及显微镜形态观察法对多组分体系分子间的相互作用和相容性进行表征分析。研究结果表明,SPI/PU具有部分相容性,而PAN/SPI、PAN/PU的相容性差,但仍然存在弱的分子间相互作用。PAN/SPI/PU体系有明显相分离现象,体系相容性差。合成制备了丙烯腈─大豆分离蛋白接枝共聚物(AN-g-SPI)和水解聚丙烯腈(HPAN)作为相容剂,随AN-g-SPI、HPAN含量增加共混膜的力学性能改善。
流变性能直接影响着纤维的纺丝成型过程和所制备纤维的结构性能。实验结果发现SPI在DMSO/Urea中剪切变稀,随浓度增加,由于其分散状态发生变化,则流动行为差异加大。原液浓度影响共混溶液的流动和成丝性,当含固量为23%时,纺丝原液的成丝性最好。SPI和PU对PAN流变性能的影响相反,SPI的加入降低了PAN溶液流动性,PAN/SPI溶液的非牛顿指数随SPI含量增加呈下降趋势,结构粘度指数则呈增加趋势。PAN/SPI/PU多组分体系的流变性能受SPI和PU含量的影响较大,可通过调整组分改变流动行为。SPI和PU的加入降低了PAN/DMSC溶液对温度的敏感性,升温有助于改善体系的流动性。
PAN/SPI/PU纤维成型机理的研究中主要探讨了凝固浴浓度和温度、拉伸比的分配比例和倍数、干燥致密化的温度和时间、交联剂的种类和浓度对其成型及性能的影响。实验结果表明:凝固浴浓度60%、温度22℃,预拉伸倍数1.5-2倍,纤维拉伸性能好。120℃干燥致密化15-20min可得强度高而干燥致密化时间也合适的纤维。采用在凝固浴中添加交联剂的方法以改善PAN/SPI纤维的性能。比较乙二醛和戊二醛的作用后,发现乙二醛加入可明显改善纤维拉伸性能,纤维拉伸强度提高近2倍,随乙二醛浓度提高纤维性能提高,但浓度超过10%后改善作用不明显。
利用红外光谱、蛋白酶水解法、表面接触角、回潮率、DSC、TGA、力学性能测试、酸性染料染色等方法对PAN/SPI/PU纤维结构性能分析表征显示:PAN/SPI/PU纤维中确实含有PAN、SPI和PU共同的特征吸收峰,然而在实验范围内蛋白酶水解法发现所测纤维中的蛋白质含量比理论添加量少。随SPI含量的增加,纤维热分解起始和峰值温度略向低温方向移动;具有部分生物降解性能;酸性染料染色性能提高;纤维的表面接触角减小,吸湿性提高。
Soy protein isolated (SPI) has been considered recently as an alternative to petroleum polymer in the manufacture of adhesives, plastics, textiles et al. Soy protein is available from renewable resources and biodegradable. Utilizing soy protein for materials will help to solve environmental and petroleum resource problems and add value for agricultural by-products.
Polyacrylonitrile (PAN) and polyurethane (PU) are general polymer material, and they have excellent performance, respectively. Blending is an important method in polymer manufacture, which may combine the advantages of both components. In this paper, the dispersion states and rheological properties of SPI in dimethylsulphoxide/urea, miscibility, interactions and rheological properties of PAN/SPI/PU system in DMSO, structure-property relationships of PAN/SPI/PU fiber were studied.
Dimethylsulfoxide(DMSO)/urea was chosen as a mixture solvent system to dissolve soy protein. The dispersion status and properties of SPI in DMSO/urea were studied. The result showed that SPI has relatively high solubility in DMSO/urea mixture solvent and urea served as a key factor of dissolving SPI in the system. The solubility properties and gelation phenomenon of SPI were studied in DMSO/Urea. The effects, such as heating time, temperature and concentration of urea were discussed. SPI in the DMSO/urea mixture system exhibited different dispersion statuses with increasing of SPI content.
Miscibility and interaction properties of PAN/SPI blend systems were studied by using methods of fourier transform infrared(FTIR), heat of mixing, dilute solution viscometry, phase contrast microscope. It was found that SPI/PU was partly miscilbility system and PAN/SPI, PAN/PU was immiscible system respectively, however there existed attractive interaction. In order to promote the compatibility, the main products of graft copolymerization of acrylonitrile and SPI (AN-g-SPI) and the alkaline hydrolysis polyacrylonitrile (HPAN) were used as the compatibilizers, and the mechanical properties of blends were improved observably.
The SPI dispersed system in DMSO/Urea was shear-thinning fluid and flow behavior was different with increasing content of SPI because the change of dispersed state. The effects of SPI and PU on the rheological properties of PAN solutions were opposite. The Non-Newtonian index of PAN/SPI solutions decreased and corresponding structure viscosity index of that increased with increasing of SPI content on the whole. The fluid properties of PAN solution was worsened with the addition of SPI. The rheological properties of PAN/SPI/PU solutions were affected by the contents of SPI and PU. In any case, the increase of temperature contributed to the improvement of the fluid properties of blend solutions.
The effect of temperature and concentration of coagulation bath, the multiple and corresponding distributive proportion of multiple drawing, temperature and time of drying, the type and concentration of crosslink agent on the properties of blend fiber were investigated. The result shown it was better to get good performance fibres when the concentration of coagulating agent was 60%, and the temperature of coagulation bath was 22℃, the drawing multiple in washing bath was 1.5-2 and the drying time was 15-20 minutes at 120℃.The effect of glutaraldehyde and glyoxal as cross-linking agent at coagulation bath on PAN/SPI fiber were studied. It was found that the mechanical properties of fibres used by glyoxal were improved.
The methods of fourier transform infrared(FTIR), enzymatic hydrolysis, scanning electron microscopy(SEM), differential scanning calorimetry (DSC), thermal gravimetric analysis (TGA), mechanical property, dye adsorption, contact angle and moisture regain measurements were employed to investigate the structure and properties of PAN/SPI/PU fiber. The results show that the concentration of SPI in PAN/SPI/PU fibers determinately increased with increasing of addition SPI by using enzymatic hydrolysis though there was loss of SPI content compared with addition of SPI weight. The PAN/SPI/PU fibers were partly biodegrability system. The thermo degraded temperature slightly decreased with increasing of content of SPI in the PAN/SPI fiber. The dye adsorption for acidic dye and moisture regain of PAN/SPI fibers increased and the contact angle of that decreased with increasing of SPI ratio as well as compared with a referenced PAN fiber prepared via the same method.
引文
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