Institute of Functional Textiles and Advanced Materials, National Engineering Research Center for Advanced Fire-Safety Materials D & A (Shandong), College of Textiles & Clothing, Qingdao University, Qingdao 266071, China.
Int J Mol Sci. 2023 Jan 24;24(3):2301. doi: 10.3390/ijms24032301.
Flame-retardant cycloaliphatic epoxy systems have long been studied; however, the research suffers from slow and unsatisfactory advances. In this work, we synthesized a kind of phosphorus-containing difunctional cycloaliphatic epoxide (called BCEP). Then, triglycidyl isocyanurate (TGIC) was mixed with BCEP to achieve epoxy systems that are rich in phosphorus and nitrogen elements, which were cured with 4-methylhexahydrobenzene anhydride (MeHHPA) to obtain a series of flame-retardant epoxy resins. Curing behaviors, flame retardancy, thermal behaviors, dielectric performance, and the chemical degradation behaviors of the cured epoxy system were investigated. BCEP-TGIC systems showed a high curing activity, and they can be efficiently cured, in which the incorporation of TGIC decreased the curing activity of the resin. As the ratio of BCEP and TGIC was 1:3, the cured resin (BCEP-TGIC) showed a relatively good flame retardancy with a limiting oxygen index value of 25.2%. In the cone calorimeter test, they presented a longer time to ignition and a lower heat release than the commercially available cycloaliphatic epoxy resins (ERL-4221). BCEP-TGIC systems presented good thermal stability, as the addition of TGIC delayed the thermal weight loss of the resin. BCEP-TGIC had high dielectric performance and outperformed ERL-4221 over a frequency range of 1 HZ to 1 MHz. BCEP-TGIC could achieve degradation under mild conditions in an alkali methanol/water solution. Benefiting from the advances, BCEP-TGIC systems have potential applications as electronic packaging materials in electrical and electronic fields.
阻燃脂环族环氧体系一直以来都受到广泛研究，但该领域的研究进展较为缓慢，不尽人意。在本工作中，我们合成了一种含磷双官能脂环族环氧化物（称为 BCEP）。然后，将三缩水甘油异氰尿酸酯（TGIC）与 BCEP 混合，得到富含磷和氮元素的环氧体系，并用 4-甲基六氢邻苯二甲酸酐（MeHHPA）进行固化，得到一系列阻燃环氧树脂。研究了固化行为、阻燃性能、热性能、介电性能以及固化体系的化学降解行为。BCEP-TGIC 体系表现出较高的固化活性，可高效固化，其中 TGIC 的加入降低了树脂的固化活性。当 BCEP 和 TGIC 的比例为 1:3 时，固化树脂（BCEP-TGIC）表现出较好的阻燃性能，其氧指数值为 25.2%。在锥形量热仪测试中，与市售脂环族环氧树脂（ERL-4221）相比，BCEP-TGIC 体系表现出更长的点火时间和更低的热释放速率。BCEP-TGIC 体系具有良好的热稳定性，因为 TGIC 的加入延迟了树脂的热失重。BCEP-TGIC 具有较高的介电性能，在 1 HZ 至 1 MHz 的频率范围内优于 ERL-4221。BCEP-TGIC 在碱性甲醇/水溶液中可在温和条件下实现降解。得益于这些优势，BCEP-TGIC 体系有望作为电子封装材料在电子和电气领域得到应用。
