硫元素在磷杂菲基阻燃环氧树脂中的作用
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贵州民族大学 化学与材料工程学院,贵州 贵阳 550025

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国家自然科学基金资助项目(51863004,52163001);贵州省科技计划(黔科合基础[2020]1Y211,ZK[2021]一般248,ZK[2022]216);贵州省科技计划(黔科合平台人才-CXTD[2021]005);贵州民族大学高分子复合材料工程研究中心(GZMUGCZX[2021]-01)


Effect of Sulfur Element on Flame-Retardant Epoxy Resin Based on Phosphaphenanthrene
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    摘要:

    为了探讨硫元素在磷杂菲基阻燃环氧树脂中的作用,将阻燃剂9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)和9,10-二氢-9-氧杂-10-磷杂菲-10-硫化物(DOPS)按照不同添加量分别添加至EP中,以4,4’-二氨基二苯砜(DDS)为固化剂制备阻燃复合材料。采用热重分析(TG)、极限氧指数(LOI)、垂直燃烧(UL-94)、锥形量热(CONE)、热重-红外光谱分析(TG-FTIR )和扫描电镜-X射线能量色谱分析(SEM-EDS)等手段,对比研究两种阻燃复合材料EP/DOPO和EP/DOPS的热稳定性、阻燃性能和成炭能力,并深入分析其阻燃机理。结果表明,当DOPO和DOPS的添加量均为10%时,EP/DOPO和EP/DOPS均达到UL-94 V-0级,LOI值分别为31.0%和30.6%;两种复合材料的热释放速率(HRR)、总热释放量(THR)和平均质量损失速率(av-MLR)值均低于纯EP,有效改善了EP的阻燃性能。而且,EP/DOPS的残炭量和阻燃性能均优于EP/DOPO,归因于DOPS中的P、S元素协同阻燃,能更好地促进基材脱水成炭,增强其凝聚相阻燃作用。SEM-EDS和TG-IR结果表明,EP/DOPS的成炭能力和炭层质量均优于EP/DOPO,阻燃剂DOPO和DOPS在气相和凝聚相共同发挥阻燃作用,但以气相阻燃作用为主,DOPS的凝聚相阻燃能力优于DOPO。

    Abstract:

    In order to investigate the effect of sulfur element on flame-retardant epoxy resin based on phosphaphenanthrene, flame retardants 9,10-dihydro-9-oxa-10- phosphaphenanthrene -10-oxide (DOPO) and 9,10-dihydro-9- oxa-10- phosphaphenanthrene -10-sulfide (DOPS) were added to EP according to the mass fraction of 5%, 7.5% and 10% respectively, and 4,4 '- diaminodiphenylsulfone (DDS) was used as curing agent to prepare flame retardant composites. Thermogravimetric analysis (TG), limiting oxygen index (LOI), vertical flame test (UL-94), cone calorimeter test (CONE), thermogravimetric-infrared spectroscopy analysis (TG-IR) and scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS) were used to compare the thermal stability, flame retardancy and charring properties of two Flame Retardant Composites EP/DOPO and EP/DOPS, and their flame retardancy mechanisms were analyzed. The results showed that when the addition of DOPO and DOPS was 10%, EP/DOPO and EP/DOPS reached UL-94 V-0, with LOI values of 31.0% and 30.6% respectively; The heat release rate (HRR), total heat release rate (THR) and average mass loss rate (av-MLR) of the two composites were lower than those of pure EP, which effectively improved the flame retardancy of EP. Moreover, the carbon residue and flame retardancy of EP/DOPS were better than that of EP/DOPO, which was attributed to the synergistic flame retardance of P and S elements in DOPS, which could better promote the dehydration of substrate into carbon and enhance the flame retardancy of condensed phase. SEM-EDS and TG-IR results showed that EP/DOPS had better charring ability and carbon layer quality than EP/DOPO. DOPO and DOPS had flame retardancy in both gas phase and condensed phase, but mainly in gas phase, and DOPS had better flame retardancy in condensed phase than DOPO.

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  • 收稿日期:2022-05-30
  • 最后修改日期:2022-08-02
  • 录用日期:2022-08-05
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