磷酸酯阻燃剂HDP的合成工艺及其在ABS中的阻燃作用

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采用新工艺路线合成高熔点磷酸酯阻燃剂———对苯二酚双(二苯基磷酸酯)(HDP).首先采用对苯二酚和三氯氧磷合成中间产物,再将中间产物与苯酚反应,经分离纯化得到产品HDP,收率达到90%以上,常温下为白色固体.采用傅里叶红外光谱、氢谱、磷谱和质谱测试确定了其结构.同时,研究了HDP的阻燃性,并与间苯二酚双(二苯基磷酸酯)(RDP)进行了比较,研究发现当HDP和RDP分别与成炭剂酚醛树脂(NP)按20/10比例添加到丙烯腈-丁二烯-苯乙烯(ABS)树脂中,增强了复合材料凝聚相阻燃作用,极限氧指数(LOI)有所提高.通过热重及锥形量热分析两种复合材料以及各种组分的热降解过程,阻燃剂的添加对ABS树脂的热稳定性和残炭量明显提高,而且ABS/HDP/NP复合材料的抑烟性更好;同时采用扫描电镜(SEM)和X射线能量色散谱(EDS),发现ABS/HDP/NP复合材料燃烧后成炭空隙均匀,其残炭中磷分布比ABS/RDP/NP复合材料残炭中的磷分布更加均匀.研究表明,HDP与NP互配添加到ABS中,在凝聚相阻燃作用优于RDP. High-melting phosphoric acid ester flame retardant, diphenyl phosphate (HDP), was synthesized by a new process route.At first, intermediate products of hydroquinone and phosphorus oxychloride were synthesized, then the intermediate product The product HDP was obtained after being separated and purified with the yield over 90% and white solid at room temperature.The structure of HDP was confirmed by Fourier transform infrared spectroscopy, hydrogen spectrum, phosphorus spectrum and mass spectrometry.At the same time, Flame retardancy and compared with resorcinol bis (diphenyl phosphate) (RDP). It was found that when HDP and RDP were added to acrylonitrile in a ratio of 20/10 with phenol-forming agent (NP) - butadiene - styrene (ABS) resin, the flame retardancy of the coacervates was enhanced and the limiting oxygen index (LOI) was enhanced.According to the thermogravimetric and cone calorimetric methods, The thermal stability and residual carbon content of ABS resin were significantly improved with the addition of flame retardant, and the smoke inhibition of ABS / HDP / NP composites was better. Meanwhile, SEM and X-ray diffraction Energy dispersive spectroscopy (EDS) showed that the charcoal of the ABS / HDP / / NP composites more uniform distribution of carbon in the carbon residue.Studies show that, HDP and NP interply added to ABS, flame retardant in the condensed phase is better than RDP.
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