采用还原剂-甲酸法溶解制备羊毛角蛋白质溶液
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摘要
为获得纤维溶解率高且蛋白质分子质量大的羊毛角蛋白质溶液,对溶解纤维的工艺方法进行研究和优化。在采用三羟基有机磷还原剂有效打开羊毛纤维分子内二硫键的基础上,重点研究了还原处理后羊毛纤维在甲酸溶液中的溶解状态。对纤维溶解率、角蛋白质溶液黏度和蛋白质分子质量分布等进行测试,获得还原剂-甲酸法溶解制备角蛋白质溶液的最优工艺,并分析了该角蛋白质溶液的稳定性能。结果表明:在角蛋白质溶液的最优制备工艺条件下,即预处理后的羊毛纤维质量为5 g,甲酸体积为100 mL,溶解温度为50℃,溶解时间为5 h时,羊毛纤维的溶解率为65%左右,角蛋白质的分子质量分布主要集中在40～50 ku、26 ku、14.4 ku处,且在常温环境下该羊毛角蛋白质溶液的稳定性较好。
In order to obtain the wool keratin solution with high fiber dissolution ratio and large protein molecular weight, the dissolution method of wool fibers was studied and optimized. On the basis of using organic phosphonic compounds(LKS-610) to effectively cleave the disulfide bonds in fibers, the dissolution state of pre-treated wool fibers in formic acid solution was studied. The fibers dissolution ratio, keratin solution viscosity and protein molecular weight distribution were tested as evaluation criteria, the optimal process for preparing keratin solution by using reducing agent-formic acid method was obtained, and the stability performance of keratin solution was also analyzed. The optimal dissolving process of wool fibers is that the mass of the pretreated wool fibers is 5 g, the volume of formic acid is 100 mL, the temperature is 50 ℃ and time is 5 h. Under the conditions, the dissolution ratio is about 65% and the molecular weights of keratin are distributed at 40-50 ku, 26 ku and 14.4 ku. In addition, the keratin solution shows good stability at normal temperature.
In order to obtain the wool keratin solution with high fiber dissolution ratio and large protein molecular weight, the dissolution method of wool fibers was studied and optimized. On the basis of using organic phosphonic compounds(LKS-610) to effectively cleave the disulfide bonds in fibers, the dissolution state of pre-treated wool fibers in formic acid solution was studied. The fibers dissolution ratio, keratin solution viscosity and protein molecular weight distribution were tested as evaluation criteria, the optimal process for preparing keratin solution by using reducing agent-formic acid method was obtained, and the stability performance of keratin solution was also analyzed. The optimal dissolving process of wool fibers is that the mass of the pretreated wool fibers is 5 g, the volume of formic acid is 100 mL, the temperature is 50 ℃ and time is 5 h. Under the conditions, the dissolution ratio is about 65% and the molecular weights of keratin are distributed at 40-50 ku, 26 ku and 14.4 ku. In addition, the keratin solution shows good stability at normal temperature.
引文
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[7] ALUIGI A, ZOCCOLA M, VINEIS C, et al. Study on the structure and properties of wool keratin regenerated from formic acid [J]. International Journal of Biological Macromolecules, 2007, 41(3): 266.
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[9] SVAGERA Z, HANZL K D, SIMEK P, et al. Study of disulfide reduction and alkyl chloroformate derivatization of plasma sulfur amino acids using gas chromatography-mass spectrometry [J]. Analytical & Bioanalytical Chemistry, 2012, 402(9): 2953.
[10] 高普, 刘建勇. TCEP羊毛低温染色助剂的性能 [J]. 印染, 2012, 38(17): 12-16.GAO Pu, LIU Jianyong. Properties of TECP for low temperature dyeing of wool fabric[J]. China Dyeing & Finishing, 2012, 38(17): 12-16.
[11] 湛海玲, 郭艺雯, 于伟东. 基于还原法的羊毛溶解及其效果表征 [J]. 纺织学报, 2009, 30(10): 37-40.ZHAN Hailing, GUO Yiwen, YU Weidong. Wool dissolution based on reduction method and characterization of its effect[J]. Journal of Textile Research, 2009, 30(10): 37-40.
[12] 王江波, 刘建勇, 王洁, 等. 基于新型还原剂羊毛角蛋白的高效溶解 [J]. 材料导报, 2012, 26(6): 7-9.WANG Jiangbo, LIU Jianyong, WANG Jie, et al. The efficent dissolution of wool based on new reductant[J]. Materials Review, 2012, 26(6): 7-9.
[13] TONIN C, ALUIGI A, VINEIS C, et al. Thermal and structural characterization of poly(ethylene-oxide)/keratin blend films [J]. Journal of Thermal Analysis & Calorimetry, 2007, 89(2): 601-608.
[14] HILL P, BRANTLEY H, VAN D M. Some properties of keratin biomaterials: kerateines [J]. Biomaterials, 2010, 31(4): 585-593.
[2] 孙艳丽, 姚金波, 李博, 等. 羊毛角蛋白质溶液的离子液体法制备 [J]. 纺织学报, 2015, 36(5): 59-62.SUN Yanli, YAO Jinbo, LI Bo, et al. Preparation of wool keratin solution with ionic liquid[J]. Journal of Textile Research, 2015, 36(5): 59-62.
[3] 张恒, 李戎, 王魁, 等. 还原法与离子液体溶解法制备羊毛角蛋白膜 [J]. 纺织学报, 2015, 36(6): 55-59.ZHANG Heng, LI Rong, WANG Kui, et al. Preparation of wool keratin membranes prepared by ionic liquid method and reduction C method[J]. Journal of Textile Research, 2015, 36(6): 55-59.
[4] SHAVANDI A, CARNE A, BEKHIT A A, et al. An improved method for solubilisation of wool keratin using peracetic acid [J]. Journal of Environmental Chemical Engineering, 2017, 5(2): 1977-1984.
[5] ZHU H, LI R, WU X, et al. Controllable fabrication and characterization of hydrophilic PCL/wool keratin nanonets by electronetting [J]. European Polymer Journal, 2017, 86:154-161.
[6] XU H, MA Z, YANG Y. Dissolution and regeneration of wool via controlled disintegration and disentanglement of highly crosslinked keratin [J]. Journal of Materials Science, 2014, 49(21): 7513-7521.
[7] ALUIGI A, ZOCCOLA M, VINEIS C, et al. Study on the structure and properties of wool keratin regenerated from formic acid [J]. International Journal of Biological Macromolecules, 2007, 41(3): 266.
[8] FAN J, YU W D. Investigation in the swelling and disintegration of wool fiber in formic acid [J]. Journal of Xi′an Polytechnic University, 2009, 23(2):310-314.
[9] SVAGERA Z, HANZL K D, SIMEK P, et al. Study of disulfide reduction and alkyl chloroformate derivatization of plasma sulfur amino acids using gas chromatography-mass spectrometry [J]. Analytical & Bioanalytical Chemistry, 2012, 402(9): 2953.
[10] 高普, 刘建勇. TCEP羊毛低温染色助剂的性能 [J]. 印染, 2012, 38(17): 12-16.GAO Pu, LIU Jianyong. Properties of TECP for low temperature dyeing of wool fabric[J]. China Dyeing & Finishing, 2012, 38(17): 12-16.
[11] 湛海玲, 郭艺雯, 于伟东. 基于还原法的羊毛溶解及其效果表征 [J]. 纺织学报, 2009, 30(10): 37-40.ZHAN Hailing, GUO Yiwen, YU Weidong. Wool dissolution based on reduction method and characterization of its effect[J]. Journal of Textile Research, 2009, 30(10): 37-40.
[12] 王江波, 刘建勇, 王洁, 等. 基于新型还原剂羊毛角蛋白的高效溶解 [J]. 材料导报, 2012, 26(6): 7-9.WANG Jiangbo, LIU Jianyong, WANG Jie, et al. The efficent dissolution of wool based on new reductant[J]. Materials Review, 2012, 26(6): 7-9.
[13] TONIN C, ALUIGI A, VINEIS C, et al. Thermal and structural characterization of poly(ethylene-oxide)/keratin blend films [J]. Journal of Thermal Analysis & Calorimetry, 2007, 89(2): 601-608.
[14] HILL P, BRANTLEY H, VAN D M. Some properties of keratin biomaterials: kerateines [J]. Biomaterials, 2010, 31(4): 585-593.