采用9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)与甲基丙烯酸-β-羟乙酯(HEMA)反应合成2-甲基-3-(6-氧代-6H-二苯并[c,e][1,2]氧磷杂己环-6-基)丙酸2-羟乙酯(DOPOHM),以 ZnB 与 DOPOHM掺杂丙烯酸树脂(AR)中,制备ZnB/膦掺杂丙烯酸树脂(ZnB-DOPOHM/AR)阻燃复合材料。利用 TGA、极限氧指数测定仪研究 ZnB-DOPOHM/AR 复合材料的热稳定性和阻燃性能；SEM,XPS 和 EDS 研究协同阻燃机制；通过Horowitz-Metzger理论计算复合材料的分解活化能(Ea )。研究表明：随着 ZnB含量增加,ZnB-DOPOHM/AR 的热稳定性提高,极限氧指数增大；ZnB 与 DOPOHM使 ZnB-DOPOHM/AR 在空气和氮气中灼烧炭层更加致密。阻燃机制揭示膦催化聚合物脱水成炭过程发生在ZnB分解产物ZnO和B2 O3表面,过程产物ZnO-P2 O5证明存在协同作用。分解活化能计算结果说明ZnO和B2 O3存在正向助催化作用,协同膦增强 ZnB-DOPOHM/AR复合材料成炭能力。
A novel flame retardant containing phosphorous 2-methyl-3-(10-oxo-10H-9-oxa-10λ5-phospha-phenan-thren-10-yl)-propionic acid 2-hydroxy-ethyl ester(DOPOHM)was synthesized by 9-oxa-10-phospha-phenanthr ene 10-oxide(DOPO)and hydroxyethyl methacrylate (HEMA),and the flame retardant materials (ZnB-DOPOHM/AR)via were prepared via DOPOHM and various of ZnB adding into acrylate resin(AR).The thermal stability and flame retardant level of composites was characterized by TGA and LOI test.The synergies mechanism between DOPOHM and ZnB was studied by SEM,XPS and EDS.The degradation activation energies(Ea)of composites were calculated by Horowitz-Metzger theory.The results indicate that the thermal stability and LOI of composites is improved by ZnB content increasing.Moreover,the char layer after combustion become more compact and smooth due to effects of both two additives.The synergies mechanism reveal that progress of catalysis effect of decomposed phosphine on matrix occur on the surface of ZnO and B2 O3 produced by ZnB,which is verified by ZnO-P2 O5 exist-ence.The calculated results show that ZnO and B2 O3 positive catalytic role and synergic phosphine-catalyzed rein-force capability of char produced.
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