磷酸乙基新戊二醇酯的合成以及阻燃性能测试

Synthesis and Flame retardancy of ethyl neopentyl phosphate

摘要:

以新戊二醇、三氯氧磷、乙醇为原料合成一种阻燃剂磷酸乙基新戊二醇酯（化合物Ⅱ），采用傅里叶变换红外光谱(IR)、核磁共振波谱(1HNMR、13CNMR及31PNMR)、液相色谱-质谱(ESI-MS)表征其化学结构。考察了物质的量比〔n(新戊二醇磷酰氯):n(乙醇)〕、反应温度和反应时间等因素对反应的影响，得到最佳反应条件为：n(新戊二醇磷酰氯) : n(乙醇)= 1.0 : 5.0，反应温度为50℃，反应时间为8 h，产率达80.8%。将合成的阻燃剂磷酸乙基新戊二醇酯添加到硬质聚氨酯泡沫(RPUF)中，通过极限氧指数(LOI)、垂直燃烧(UL-94)实验测定RPUF的阻燃性能，以及利用热重分析(TGA)表征阻燃剂和RPUF的热稳定性。结果表明，磷酸乙基新戊二醇酯的添加，在一定程度上降低了RPUF的热稳定性，但是RPUF的阻燃性能有所提高。添加量为30%(质量分数，以材料总质量计)时可使RPUF的LOI值从17.1提高到22.5%，通过垂直燃烧V-2级，以及在800℃时，残余残炭量由15.8%增加到18.9%。

Abstract:

A flame retardant named as ethyl neopentyl phosphate was synthesized with neopentyl glycol, phosphorus ox-ychloride and ethanol as raw materials. The chemical structure of ethyl neopentyl phosphate was identified by means of FTIR, 1HNMR, 13CNMR, 31PNMR and ESI-MS. The effects of material ratio, reaction time and reaction temperature on the reaction were studied. The results show that the optimum conditions are (neopentyl glycol chlorophosphate):n (ethanol) = 1.0:5.0, the reaction temperature is 50℃, the reaction time is 8 h and the yield of the obtained product can reach 80.8%. Ethyl neopentyl phosphate was then applied in rigid polyurethane foams (RPUF), and the flame retardancy of the resulting composite material was determined by limiting oxygen index (LOI) measurements and vertical (UL-94) tests. Meanwhile, the thermal stability of flame retardant and RPUF was characterized by thermogravimetric analysis (TGA). The results indicated that the addition of ethyl neopentyl phosphate reduced the thermal stability to a certain extent, but improved the flame retardancy of RPUF. the composite containing 30% ethyl neopentyl phosphate could achieve UL-94 V-2 rating with a LOI value of 22.5. %, higher than that of pure RPUF(17.1%), and the residual mass increased from 15.8% ( for pure RPUF) to 18.9%.