新型阻燃剂间苯三酚三(二苯基磷酸酯)的合成及其阻燃环氧树脂研究

Synthesis of a New Phloroglucin Tri(diphenyl phosphate)Flame Retardant and Its Application in Epoxy Resins

以间苯三酚、三氯氧磷和苯酚为原料,合成了间苯三酚三(二苯基磷酸酯)(PDP)阻燃剂,并通过红外光谱分析和元素分析表征了其结构。结果表明,反应的最佳工艺条件为:无水三氯化铝作为催化剂,间苯三酚与三氯氧磷的物质的量之比为1:5;第一步反应温度为70℃,反应时间为7 h;第二步反应温度为130℃,反应时间为8 h。产品收率达87.2%。PDP 阻燃环氧树脂的应用实验表明,其与三聚氰胺质量比为3:1的复配体系添加量为15%(质量分数,下同)时,环氧树脂的氧指数为32.2%,达到 UL94 V-0级。

Phloroglucin tri （diphenyl phosphate） was synthesized based on phloroglucin, phosphorus oxychloride, and phenol. The optimal reaction conditions were as following： using aluminum chloride as a catalyst, molar ratio of phloroglucin to phosphorus oxychloride was 1 ： 5, reacted for 7 h at 70 ℃, followed by 8 h at 130 ℃. A gross yield of 87.2 % was obtained. A mixture of the product and mdarnine （mass ratio 3：1） was introduced into epoxy resin （mass ratio of epoxy/mixture= 85/15）, the limiting oxygen index and UL94 of the latter became 32.2 % and V-0, respectively.