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通过在聚磷酸铵(APP)缩聚反应过程中加入钙基纳米蒙脱土(CaMMT),制备CaMMT/APP复合物,以提高CaMMT在APP中的分散性,并提高其热性能。采用FTIR、XRD、TGA、31P核磁共振(31P NMR)以及水溶解性和pH值测试等,表征了添加不同质量分数的CaMMT和在不同温度下制备得到的CaMMT/APP复合物的结构和性质。测试分析表明:CaMMT/APP中CaMMT是完全剥离的,表明CaMMT在APP中分散性好。随着复合物中CaMMT含量增加,复合物中Ⅰ型结晶APP比例提高,APP聚合度下降,复合物水溶性增大,起始分解温度降低,但800℃时复合物的残余质量分数更高。当CaMMT的添加量相同时,添加CaMMT时反应体系的温度越高,越有利于生成高聚合度的结晶Ⅱ型APP,复合物的水溶性也降低,热性能提高,温度为210℃,复合物在800℃的残余质量分数为29.69%,当温度为300℃时,复合物残余质量分数上升至53.75%。
The CaMMT / APP complex was prepared by adding calcium-based nano-montmorillonite (CaMMT) during polycondensation of ammonium polyphosphate (APP) to improve the dispersibility of CaMMT in APP and improve its thermal properties. The structure and properties of CaMMT with different mass fractions and CaMMT / APP complexes prepared at different temperatures were characterized by FTIR, XRD, TGA, 31P NMR and water solubility and pH values. Test analysis shows that: CaMMT / APP CaMMT is completely stripped, indicating that CaMMT good dispersion in the APP. With the increase of CaMMT content in the complex, the proportion of APP in type I crystal increased, the degree of polymerization of APP decreased, the water solubility of the complex increased, the initial decomposition temperature decreased, but the residual mass fraction of the complex was higher at 800 ℃. When the amount of CaMMT added is the same, the higher the temperature of the reaction system when CaMMT is added, the more conducive to the formation of high degree of polymerization of type Ⅱ APP, the water solubility of the composite is also reduced, the thermal properties increased, the temperature is 210 ℃, the complex The residual mass fraction at 800 ℃ was 29.69%. When the temperature was 300 ℃, the residual mass fraction increased to 53.75%.