新型含磷封端阻燃剂的合成及其对聚对苯二甲酸丁二醇酯性能的影响

Synthesis of a novel phosphorus-terminated flame retardant and its application in PBT system

以季戊四醇磷酸酯(PEPA)、三氯氧磷和1,4-丁二醇(BDO)为原料合成了一种含有磷氧螺环结构的封端阻燃剂。通过红外光谱和核磁共振谱等方法对该化合物的结构进行表征,通过热重分析评价其热稳定性,探讨了聚双季戊四醇双磷酸酯螺环丁二醇磷酸酯(PASPB)用量对聚对苯二甲酸丁二醇酯(PBT)端羧基含量的影响,并测试了其抗水解性能和与次膦酸铝复配的阻燃性能。结果表明:热重分析表明其初始分级温度为346℃,800℃时残炭率为41.11%,热稳定性良好;PASPB用量在3.5份以上时,残留的端羧基浓度已达到10mmol/kg以下,可满足PBT抗水解的基本要求:当PASPB添加量为6份,二乙基次膦酸铝添加量为9份时,阻燃复合材料的极限氧指数(LOI值)达到了30.5,拉伸强度为51.2MPa。

A novel phosphorus-containing flame retardant PASPB which used PEPA,phosphorus oxychloride and 1,4-butanediol as raw material was synthesized successfully.The structure and thermal degradation behavior of product was characterized by fourier transform spectrometry（FT-IR）,nuclear magnetic resonances（NMR）and thermal gravimetric analyzer（TG）.The effects of the amount of poly pentaerythritol phosphate spirocyclic phosphorus oxychloride spirocyclic butylene glycol（PASPB）on the carboxyl content of PBT were discussed,its anti-hydrolysis performance and the flame retardancy with the phosphinate were tested.Thermogravimetric analysis showed that the initial classification temperature was 346℃ ,the char residue rate was 41.11% at 800℃ ,and the thermal stability was good.The residual carboxyl group concentration of PASPB was above 10 mmol/kg when the amount of PASPB was over 3.5 phr,which can meet the basic requirement of hydrolysis resistance of PBT.When the amount of PASPB was 6 phr and the amount of diethylphosphinate was 9 phr,the LOI value was 30.5 and the tensile strength was 51.2 MPa.