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第 4 期 徐 洋，等: 三（2-羟丙基）磷酸酯的合成
2.2.5 热重分析
对产品进行热重分析，氮气流速 100 mL/min，
升温速率 5 ℃/min，结果见图 6。从图 6 可以看出，
产品的热分解大致分为 4 个阶段。第一阶段为
20~150 ℃，这个阶段失重主要是由于产品中少量的
水分挥发引起；第二阶段为 150~250 ℃，失重是由
于分子中较多不稳定的 P—O—C 断裂所致；第三阶
段为 250~600 ℃，失重主要是因为进一步炭化所致
第四阶段为 600~700 ℃，此时失重幅度较小。DTA
曲线在 249 ℃左右有一个放热峰，对应于 P—O—C
键断裂分解放热并伴随失重。600 ℃时，产品的残
炭率为 16.66%，比一般的磷系阻燃剂高
产品具有很好的热稳定性。
图 6 产品的 TG-DTA 曲线
Fig. 6 TG-DTA curve of product
3 结论
以磷酸、环氧丙烷为原料，在路易斯酸离子液
体催化下合成了三（3-羟丙基）磷酸酯。最佳工艺
条件为：磷酸、1,2-环氧丙烷的物质的量比为 1.0∶
3.2，反应温度为 90 ℃，反应时间为 3 h，在此条
件下得到无色半透明液体，收率为 92.8%。产物折
光率为 1.4340，酸值为 0.06 mg KOH/g，黏度为 85
mPa·s（25 ℃），磷元素质量分数为 11.5%，羟值为
615 mg KOH/g。该合成方法条件温和，原子经济性
高，由于羟基的存在，三（3-羟丙基）磷酸酯可以
作为反应型阻燃剂，其在聚氨酯泡沫中不易析出，
效果持久。
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