新型环三磷腈衍生物的合成及表征

Synthesis and Characterization of a Novel Cyclotriphosphazene Derivative

以六氯环三磷腈(HCCP)、新戊二醇(NPG)和金属钠为原料,制备一种新型环三磷腈阻燃剂三(2,2-二甲基-1,3-丙二氧基)环三磷腈(TDPCP)。采用傅里叶红外光谱、核磁共振氢谱、核磁共振磷谱、元素分析和热重对产物的结构和热性能进行了表征,并探究了反应溶剂、反应物投料比、反应温度和反应时间对TDPCP收率的影响。结果表明:以四氢呋喃为溶剂,n(HCCP)∶n(NPG)=1∶4.5,70℃回流反应24 h,TDPCP收率可达85.5%;产物结构与TDPCP相一致;TDPCP的初始分解温度为243℃,800℃的残碳量为14.6%,是一种耐热性和稳定性较好的杂环化合物。

A novel cyclotriphosphazene derivative,tri（2,2-dimethyl-1,3-dioxole） cyclotriphos-phazene（TDPCP）was prepared using hexachlorocyclotriphosphazene（HCCP）, neopentyl glycol（NPG） and sodium as raw materials.The chemical structure and thermal property of TDPCP were characterized by Fourier infrared spectroscopy,nuclear magnetic resonance, element analysis, thermogravimetric analysis and derivative thermogravimetricanalysis. The effects of solvent, feed mole ratio, reaction temperature and time on the yield of TDPCP were alsoinvestigated. The results showed that the yield of TDPCP was 85.5% through the reaction at 70 ℃ for 24 h whenthe mole ratio of HCCP to sodium NPG dissolved in tetrahydrofuran was 1∶4.5. The initial decompositiontemperature of TDPCP was 243.47 ℃ and the amount of residual carbon was 14.6% at 800 ℃, indicating thatTDPCP is a heterocyclic compound with good heat resistance and stability.