一种新型P-N-Cl协效阻燃剂的合成及其在热固性树脂中的应用

Synthesis of a New Type Benzimidazole Flame Retardant with P-N-Cl Synergistic Effect and Its Application in Thermosetting Resin

以邻苯二胺、顺丁烯二酸和三氯氧磷为原料,以三乙胺作为缚酸催化剂,合成了新型P-N-Cl协效苯并咪唑型阻燃剂。利用元素分析、FTIR及1H NMR波谱对中间体和阻燃剂分子结构进行了表征。通过单因素实验考察了反应时间、反应温度及原料物质的量比nPOCl3∶n中间体(I)等主要反应条件对P-N-Cl协效阻燃剂收率的影响,发现在t=8 h,T=75℃以及nPOCl3∶n中间体(I)=2.25的优化条件下,阻燃剂最大收率为73.6%。通过极限氧指数(LOI)测定,考察了该P-N-Cl协效阻燃剂对191型不饱和树脂和环氧树脂E-44的阻燃效果,结果发现在阻燃剂质量分数12%时二者的LOI可分别达到33.7%和32.3%,表明其具有良好的阻燃性能和潜在应用前景。

A benzimidazole type flame retardant with P-N-Cl synergistic effect was synthesized using o-phenylenediamine,maleic acid,phosphorus trichloride as raw material and triethylamine as catalyst.The intermediate and target flame retardant were characterized by means of elemental analyses,FTIR and 1H NMR spectra.The effects of reaction time,reaction temperature and n POCl3∶nintermediate （Ⅰ） on the yield of P-N-Cl synergistic effect flame retardant were investigated by single factor experiment.The results showed that the highest yield 73.6％ can be obtained under the optimum reaction conditions：reaction time 8 h,reaction temperature 75 ℃ and nPOCl3∶ni diate （Ⅰ） =2.25∶1.The LOI （limit oxygen index） test was carried out to evaluate the fire retarding performance of the products for unsaturated resin 191 and epoxy resin E-44.The LOIs for the unsaturated resin （191） and epoxy resin （E-44） reached 33.7％ and 32.3％ respectively when the flame retardant contained 12％.The results indicated that the P-N-C1 synergistic flame retardant had good flame retardant effect and potential application prospects.