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高聚合度聚磷酸铵中特征磷的31P核磁共振分析

Analysis of Characteristic Phosphorus in High Polymerization Ammonium Polyphosphate by 31p NMR

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【作者】 刘宜娜杨荣杰HU Weiguo李定华

【Author】 LIU Yina;YANG Rongjie;HU Weiguo;LI Dinghua;Scholl of Materials Science and Engineering,National Engineering Research Center of Flame Retardant Materials,Beijing Institute of Technology;Department of Polymer Science & Engineering,University of Massachusetts Amherst;

【通讯作者】 杨荣杰;

【机构】 北京理工大学材料学院国家阻燃材料工程技术研究中心Department of Polymer Science & Engineering,University of Massachusetts Amherst

【摘要】 采用一维31p核磁共振(31p NMR)、二维J分解谱(J-resolved)和扩散核磁(31p DOSY)等方法,研究了高聚合度聚磷酸铵(APP)和多聚磷酸盐的特征磷及其偶合常数.研究表明,多聚磷酸盐及其中所含的二聚磷酸盐端基磷分别呈双峰和单峰特征,多聚磷酸盐自旋偶合裂分的端基磷共振峰的偶合常数为19.4 Hz. APP中含有小分子二聚磷酸铵和正磷酸铵,用31p NMR定量表征APP聚合度时需排除二聚体端基磷峰的面积.在100℃水中溶解APP制备的APP水溶液中,部分高聚合度APP发生断链,中间磷共振峰处出现短链APP的磷共振峰.

【Abstract】 In this paper,phosphorus nuclear magnetic resonance(31p NMR),J-resolved and 31p-DOSY are used to study the characteristic phosphorus and coupling constants of APP. Studies have shown that the endgroup phosphors of polyphosphate and diphosphate have double-peak and single-peak characteristics respectively,and the coupling constant of spin-coupled peak is 19.4 Hz;Ammonium phosphate(Ⅱ-APP)contains ammonium di-polyphosphate and ammonium orthophosphate. When 31p NMR is used to quantitatively characterize the degree of APP polymerization,the terminal phosphorus of ammonium di-polyphosphate should be excluded;when APP is prepared by dissolving APP in water at 100 ℃,the appearance of the phosphorus resonance peak of small molecule middle phosphorus proves that APP has partially broken chain.

  • 【文献出处】 高等学校化学学报 ,Chemical Journal of Chinese Universities , 编辑部邮箱 ,2020年12期
  • 【分类号】O657.2;TQ314.248
  • 【被引频次】1
  • 【下载频次】232
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