New flame retardant epoxy resins based on cyclophosphazene-derived curing agents

• Published in: Chinese chemical letters 2022-08, Vol.33 (8), p.4026-4032
• Main Authors: Miao, Zhenwei, Yan, Dongpeng, Wang, Xiaodong, Zhang, Xinfang, Zhou, Wenqi, Qiu, Munan, Yang, Fan, Wu, Zhanpeng
• Format: Article
• Language: English
• Subjects: Curing agent; Cyclotriphosphazene; Epoxy resin; Flame retardancy; Pyrolysis mechanism
• ISSN: 1001-8417; 1878-5964
• DOI: 10.1016/j.cclet.2021.12.003

To obtain high-efficiency flame retardancy of epoxy resins, a cyclophosphazene derivative tri-(o-henylenediamino)cyclotriphosphazene (3ACP) was successfully synthesized and used as a curing agent for the thermosetting of an epoxy resin system. The flame retardant properties, thermal stability, and pyrolysis mechanism of the resultant thermosets were investigated in detail. The experiments indicated that the synthesized thermoset achieved a UL-94 V-0 rate under a vertical burning test as well as a limiting oxygen index (LOI) of 29.2%, which was able to reach V-0 even when a small amount of 3ACP was incorporated. Scanning electronic microscopic observation demonstrated that the char residue of the thermosets was extremely expanded after the vertical flame test. Thermal analysis showed that the samples had a lower initial decomposition temperature when 3ACP was introduced into the epoxy resin systems. This indicates that the carbonization ability of the thermosets was significantly improved at elevated temperatures. In addition, the incorporation of 3ACP can effectively suppress the release of combustible gases during the pyrolysis process, and the decomposition of E-44/DDS-3ACP curing systems also promotes the formation of polyphosphoramides charred layer in the condensed phase. The investigation on the chemical structures of both the gaseous and condensed phase pyrolysis process confirmed the flame-retardant mechanism of the 3ACP-cured epoxy resins. Therefore, the nonflammable halogen-free epoxy resin developed in this study has potential applications in electric and electronic fields for environment protection and human health. Novel reactive flame retardant additive (3ACP) is used to prepare epoxy resin curing system which obtains self-extinguishing properties and elevated LOI value. [Display omitted]