赛克改性三聚氰胺甲醛树脂的合成及协效阻燃作用

Synthesis and Synergistic Flame Retardancy of the Melamine Formaldehyde Resin Modified with THEIC

采用固相合成法,通过六羟甲基三聚氰胺(HMM)与赛克醚化和缩聚合成了赛克改性三聚氰胺甲醛树脂(简称赛改树脂),并通过红外光谱和固体13C NMR表征了其结构。其较佳的合成条件:n(HMM)∶n(赛克)=1∶2.50,反应温度130℃,反应时间4 h。在此条件下,产品的质量产率为86.2%,水溶性为0.177 g·(100 mL)^(-1)水;赛克树脂的初始热稳定性、成炭能力和对聚丙烯(PP)的协效阻燃作用均好于HMM和赛克,例如HMM、赛克和赛改树脂的T5%分别为149、245和291℃,750℃时的残余率分别为9.48%、0.30%和12.14%,阻燃PP达到V-0级时,聚磷酸铵(APP)/赛改树脂、APP/HMM和APP/赛克的最小添加量分别为24%、34%和26%。PP/APP/赛改树脂的耐水性也明显好于PP/APP/赛克。

The melamine formaldehyde resin modified with THEIC(resin modified with THEIC in brief)was synthesized through the etherification and condensation of hexahydroxymethyl melamine(HMM)with THEIC by using solid phase synthesis method,and its structure was characterized by infrared spectroscopy and solid 13 C NMR.The better synthesis conditions were as follows:n(HMM)∶n(THEIC)=1∶2.50,reaction temperature being 130℃and reaction time being 4 h.Under the above conditions,the mass yield of the product was 86.2%and the water solubility was 0.177 g·(100 mL)^(-1).The initial thermal stability,charring ability and synergistic flame retardancy in polypropylene(PP)of the resin modified with THEIC are better than those of HMM and THEIC,for example,the T5%of HMM,THEIC and the resin are 149,245 and 291℃,respectively,and the residual at 750℃is 9.48%,0.30%and 12.14%,respectively,when the flame retardant PP reaches V-0 level,the minimum of ammonium polyphosphate(APP)/the resin,APP/HMM and APP/THEIC were 24%,34%and 26%,respectively.The water resistance of PP/APP/the resin is also significantly superior to that of PP/APP/THEIC.