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  

Process Optimization for Ball Milling-assisted Degradation of Sodium Alginate as Well as Its Structure and Property

作　　者：李正月 李东泽 孙秀英 蔡沛文 廖雨青 陈秀琼 颜慧琼 林强[1,2,3] LI Zhengyue;LI Dongze;SUN Xiuying;CAI Peiwen;LIAO Yuqing;CHEN Xiuqiong;YAN Huiqiong;LIN Qiang(Key Laboratory of Water Pollution Treatment and Resource Reuse of Hainan Province,Haikou 571158,China;Key Laboratory of Natural Polymer Functional Material of Haikou City,Haikou 571158,China;Key Laboratory of Tropical Medicinal Resource Chemistry of Ministry of Education,Hainan Normal University,Haikou 571158,China)

机构地区：[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

出　　处：《材料导报》2022年第6期204-209,共6页Materials Reports

基　　金：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)。

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(M_(W))为响应值,采用Box-Behnken设计建立模型,考察球磨时间、CuCl_(2)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(^(1)H-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、CuCl_(2)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H_(2)O_(2)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。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(M_(W))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,CuCl_(2)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(^(1)H-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 CuCl_(2)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 H_(2)O_(2)and the coordination of Cu^(2+),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.

关 键 词：机械球磨法 海藻酸盐 降解 响应面法 优化 

分 类 号：O648.23[理学—物理化学]