新型磷氮阻燃剂TGICA-DOPO的合成及其对乙烯基酯树脂阻燃性能的影响

陶晓晓; 段华军; 董文静; 汪鑫

doi:10.13801/j.cnki.fhclxb.20171026.002

新型磷氮阻燃剂TGICA-DOPO的合成及其对乙烯基酯树脂阻燃性能的影响

Preparation of a novel flame retardant TGICA-DOPO and its effects on the properties of vinyl ester resin

摘要

摘要: 以异氰尿酸三缩水甘油酯（TGIC）、丙烯酸和9，10-二氢-9-氧杂-10-磷杂菲-10-氧化物（DOPO）为主要原料，合成了一种含P和N元素的新型阻燃添加剂TGICA-DOPO，将其应用在乙烯基酯树脂（VER）中可以制备具有良好阻燃性能的TGICA-DOPO/VER复合材料。通过FTIR光谱、核磁共振（³¹P-NMR和¹H-NMR）等对TGICA-DOPO的分子结构进行了表征；通过极限氧指数（LOI）测试、TGA和DMA研究了TGICA-DOPO/VER树脂体系的阻燃性能和耐热性能。结果表明，当树脂体系中TGICA-DOPO的质量分数为30wt%时，LOI达到35；当体系中TGICA-DOPO的质量分数为25wt%时，树脂浇铸体在800℃下的残炭量提高了322%；FTIR和SEM测试结果表明，燃烧时TGICA-DOPO有助于形成高致密、连续炭层，隔绝了热量和空气向基材的传递，从而在凝聚相中发挥阻燃作用。

Abstract: A novel flame retardant containing P and N was successfully synthesized via the addition reaction between triglycidyl isocyanurate (TGIC), acrylic acid and 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO). A flame retardant composite material TGICA-DOPO/vinyl ester resin (VER) was prepared by applying it to VER. The structure of TGICA-DOPO is characterized by FTIR, ¹H and ³¹P nuclear magnetic resonance (NMR). The flame retardancy and thermal properties of TGICA-DOPO/VER resin system were respectively investigated by limited oxygen index (LOI) measurement, TGA and DMA. The results show that the LOI value of the resin system containing 30wt% TGICA-DOPO is improved to 35. TGA results indicate that the char yields of VER casting containing 25wt% TGICA-DOPO under 800℃ is increased by 322%. The FTIR and SEM results indicate that TGICA-DOPO promotes the formation of continuous, compact and intumescent char layer which can reduce the efficiency of heat-and oxygen-exchange.

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