Preparation of halogen-free flame retardant curing agent and its application in epoxy resin

Abstract

9,10-Dihydro-9-oxa-10-phosphaphenanthrene-10-oxide-N-Aminoethylpiperazine (DOPO-AEP), a phosphorus and nitrogen intumescent flame retardant curing agent was prepared by using acetonitrile as solvent using 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and N-aminoethylpiperazine (AEP) as raw materials. The structure of the flame retardant curing agent DOPO-AEP was analyzed Fourier Transform Infrared Spectrometer (FTIR), Nuclear Magnetic Resonance (NMR) and Electrospray Ionization Mass Spectrometry (ESI-MS), and the synthesis method of the target product was determined. In addition, the content of char residue was determined by thermogravimetric analyzer, and its thermal properties were comprehensively explored, and based on the obtained results, the curable epoxy resin was selected to prepare DOPO-AEP/EP flame retardant composites. According to the amount of DOPO-AEP added product, different proportions of DOPO-AEP/EP flame retardant composites were prepared, and the actual impact of flame retardant properties and mechanical properties of epoxy resin in different proportions was explored. When the content of DOPO-AEP is 35%, the limiting oxygen index of DOPO-AEP/EP reaches 29.9, which has a significant increase compared with the limiting oxygen index of pure epoxy resin of 19.8, but compared with the content of DOPO-AEP of 30%, the limiting oxygen index of DOPO-AEP/EP is 28.7, and there is no significant increase change. Comprehensive analysis shows that when the component content of DOPO-AEP is 30%, the flame retardant system has a tensile strength of 29.0 MPa, an impact strength of 4.5Kj/m² and a flexural strength of 73.9 MPa, and its limiting oxygen index is as high as 28.7, and the comprehensive performance of the system is the best. By testing the surface morphology of the flame retardant composites after combustion by SEM, it was found that a dense char layer was formed on the surface of the epoxy resin cured char residue and foamed obviously, indicating that the flame retardant curing performance of DOPO-AEP was good.