| 高聚合度聚磷酸铵中特征磷的31P核磁共振分析 |
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| 引用本文： | 刘宜娜,杨荣杰,HUWeiguo,李定华.高聚合度聚磷酸铵中特征磷的31P核磁共振分析[J].高等学校化学学报,2020,41(12):2832. |
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| 作者姓名： | 刘宜娜 杨荣杰 HUWeiguo 李定华 |
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| 作者单位： | 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 |
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| 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.
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| 关 键 词： | 聚磷酸铵 核磁共振 特征磷 聚合度 |
| 收稿时间： | 2020-06-17 |
Analysis of Characteristic Phosphorus in High Polymerization Ammonium Polyphosphate by 31P NMR |
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| LIU Yina,YANG Rongjie,HU Weiguo,LI Dinghua.Analysis of Characteristic Phosphorus in High Polymerization Ammonium Polyphosphate by 31P NMR[J].Chemical Research In Chinese Universities,2020,41(12):2832. |
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| Authors: | LIU Yina YANG Rongjie HU Weiguo LI Dinghua |
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| Institution: | 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 |
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| 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. |
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| Keywords: | Ammonium polyphosphate Nuclear magnetic resonance Characteristic phosphorus Degree of polymerization（Ed ： W Z M） |
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