网状结构结晶Ⅴ型聚磷酸铵的合成与表征

Synthesis and Characterization of Reticulated Structure Ammonium Polyphosphate with Crystal Form Ⅴ

以质量分数为85%的食品级磷酸为原料,以三聚氰胺为缩合剂,合成了一种具有网状结构的结晶Ⅴ型聚磷酸铵,对其水溶性、XRD、13CNMR、红外光谱及热重等进行了测试与表征,并与结晶Ⅰ型和结晶Ⅱ型产品进行了对比.结果表明,所制得的产品具有良好的耐水性,其XRD图谱与结晶Ⅴ型完全一致.13CNMR及红外图谱表明,该物质是以三嗪环为基本骨架的聚磷酸铵链交联网状结构.热重分析表明,在700℃时该产品残重为53.6%,大于结晶Ⅰ型(40.29%)和结晶Ⅱ型(36.16%),初步显示该产品具有良好的高温热稳定性.

Ammonium polyphosphate（APP） with reticulated structure was prepared by heating a mixture of 85%（mass fraction） food grade phosphoric acid and melamine under wet ammonia atmosphere.Its water-solubility,XRD,13C NMR,FTIR and TG were investigated,and compared with those of APP-Ⅰ and APP-Ⅱ.The results show that this product has excellent water-resistence,its XRD spectrum is similar to that of APP-Ⅴ in literature,its 13C NMR and FTIR spectra show that this product is a cross-linked and reticulated structure of ammonium polyphosphate chains with triazine ring as basebone.TG tests show that the residual mass fraction at 700 ℃ for this product is 53.6%,higher than 40.29% for APP-I and 36.16% for APP-Ⅱ,meaning its excellent thermal stability at high temperature.