高等学校化学学报 ›› 2020, Vol. 41 ›› Issue (12): 2832-2837.doi: 10.7503/cjcu20200365

• 高分子化学 • 上一篇    下一篇

高聚合度聚磷酸铵中特征磷的31P核磁共振分析

刘宜娜1, 杨荣杰1(), HUWeiguo2, 李定华1   

  1. 1.北京理工大学材料学院, 国家阻燃材料工程技术研究中心, 北京 100081
    2.Department of Polymer Science & Engineering, University of Massachusetts Amherst, MA 01003, USA
  • 收稿日期:2020-06-17 出版日期:2020-12-10 发布日期:2020-12-09
  • 通讯作者: 杨荣杰 E-mail:yrj@bit.edu.cn

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

LIU Yina1, YANG Rongjie1(), HU Weiguo2, LI Dinghua1   

  1. 1.Scholl of Materials Science and Engineering,National Engineering Research Center of Flame Retardant Mate? rials,Beijing Institute of Technology,Beijing 100081,China
    2.Department of Polymer Science & Engineering,University of Massachusetts Amherst,MA 01003,USA
  • Received:2020-06-17 Online:2020-12-10 Published:2020-12-09
  • Contact: YANG Rongjie E-mail:yrj@bit.edu.cn

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.

关键词: 聚磷酸铵, 核磁共振, 特征磷, 聚合度

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 end-group 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.

Key words: Ammonium polyphosphate, Nuclear magnetic resonance, Characteristic phosphorus, Degree of polymerization(Ed.: W, Z, M)

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