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材料导报  2022, Vol. 36 Issue (6): 21010003-6    https://doi.org/10.11896/cldb.21010003
  高分子与聚合物基复合材料 |
球磨辅助海藻酸钠降解工艺参数的优化及其产物的结构和性能
李正月1,2,3, 李东泽1,2, 孙秀英1,2, 蔡沛文1,2, 廖雨青1,2, 陈秀琼1,2, 颜慧琼1,2,3, 林强1,2,3
1 海南省水环境污染治理与资源化重点实验室,海口 571158
2 海口市天然高分子功能材料重点实验室,海口 571158
3 海南师范大学热带药用植物化学教育部重点实验室,海口 571158
Process Optimization for Ball Milling-assisted Degradation of Sodium Alginate as Well as Its Structure and Property
LI Zhengyue1,2,3, LI Dongze1,2, SUN Xiuying1,2, CAI Peiwen1,2, LIAO Yuqing1,2, CHEN Xiuqiong1,2, YAN Huiqiong1,2,3, LIN Qiang1,2,3
1 Key Laboratory of Water Pollution Treatment and Resource Reuse of Hainan Province, Haikou 571158, China
2 Key Laboratory of Natural Polymer Functional Material of Haikou City , Haikou 571158, China
3 Key Laboratory of Tropical Medicinal Resource Chemistry of Ministry of Education, Hainan Normal University, Haikou 571158, China
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摘要 为了促进海藻资源的开发和高效利用,采用机械球磨法辅助海藻酸钠(SA)的降解,以获得低分子量SA。以降解SA的质均分子量(MW)为响应值,采用Box-Behnken设计建立模型,考察球磨时间、CuCl2浓度和溶液pH值对响应值的影响,进而采用凝胶色谱仪(GPC)、红外光谱仪(FTIR)、核磁共振波谱仪(1H-NMR)、热重分析仪(TGA)、X射线衍射仪(XRD)对降解SA的结构和性能进行表征。结果表明,响应值与三因素关系对二次模型的拟合度较好,在试验范围内,该数学回归模型具有良好的预测性。在各因素设定范围内预测最佳工艺参数为:球磨时间94.38 min、CuCl2浓度4.00 mmol/L、溶液pH值1.43。同时,对降解SA的结构和性能的测试结果表明,由于在H2O2的强氧化作用和金属铜离子的配位作用下,SA分子链发生裂解,分子量降低,分子内氢键遭受破坏,作用力减弱,使得部分分子骨架结构发生了变化,形成了分子内酯。
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李正月
李东泽
孙秀英
蔡沛文
廖雨青
陈秀琼
颜慧琼
林强
关键词:  机械球磨法  海藻酸盐  降解  响应面法  优化    
Abstract: In order to promote the development and efficient utilization of seaweed resources, mechanical ball milling was used to assist the degradation of sodium alginate (SA) to obtain low molecular weight SA. Taking the mass average molecular weight (MW) of the degraded SA as the response value, the Box-Behnken design was used to build the model and analyze the effects of ball milling time, CuCl2 concentration and solution pH on the response value. Furthermore, the structure and performance of the degraded SA were characterized by gel chromatography (GPC), infrared spectrometer (FTIR), nuclear magnetic resonance spectrometer (1H-NMR), thermos-gravimetric analyzer (TGA) and X-ray diffracto-meter (XRD). The experimental results showed that the relationship between the response value and three independent variables were in line with the quadratic model. The mathematical regression model had good predictability and the optimal conditions within the experimental ranges for the response value were forecasted to be 94.38 min for ball milling time, 4.00 mmol/L for CuCl2 concentration, and 1.43 for solution pH. Meanwhile, the structure and performance test results of the degraded SA showed that due to the strong oxidation of H2O2 and the coordination of Cu2+, the SA was degraded, the molecular weight reduced, the intramolecular hydrogen bond was destroyed, and the force weakened. As a result, part of the molecular skeleton structure had changed, forming a molecular lactone.
Key words:  mechanical ball milling method    alginate    degradation    response surface methodology    optimization
出版日期:  2022-03-25      发布日期:  2022-03-21
ZTFLH:  O648.2+3  
基金资助: 国家自然科学基金(51963009);海南省自然科学基金(219QN209);海南省研究生创新科研课题(Hys2020-309)
通讯作者:  yanhqedu@163.com;linqianggroup@163.com   
作者简介:  李正月,2019年6月毕业于河北科技大学,获得学士学位。现为海南师范大学化学与化工学院硕士研究生,主要从事海藻多糖开发与应用研究。
颜慧琼,理学博士,副教授。2010年于海南大学化学工程与工艺学院获得学士学位,2017年7月毕业于海南师范大学化学专业并获得理学博士学位。2017年6月至今在海南师范大学化学与化工学院进行教学科研工作。主要从事缓控释农药剂型开发与应用、海藻多糖的功能化修饰以及基于海藻酸盐复合凝胶的组织工程支架材料与生物传感器的制备及应用。目前在国内外知名期刊发表论文共60余篇,其中SCI收录40余篇。申请国家发明专利 4 项,其中 3 项已授权。
引用本文:    
李正月, 李东泽, 孙秀英, 蔡沛文, 廖雨青, 陈秀琼, 颜慧琼, 林强. 球磨辅助海藻酸钠降解工艺参数的优化及其产物的结构和性能[J]. 材料导报, 2022, 36(6): 21010003-6.
LI Zhengyue, LI Dongze, SUN Xiuying, CAI Peiwen, LIAO Yuqing, CHEN Xiuqiong, YAN Huiqiong, LIN Qiang. Process Optimization for Ball Milling-assisted Degradation of Sodium Alginate as Well as Its Structure and Property. Materials Reports, 2022, 36(6): 21010003-6.
链接本文:  
http://www.mater-rep.com/CN/10.11896/cldb.21010003  或          http://www.mater-rep.com/CN/Y2022/V36/I6/21010003
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