Synthesis of a novel phosphorus and nitrogen-containing flame retardant and its application in rigid polyurethane foam with expandable graphite

• Published in: Polymer degradation and stability Vol. 173; p. 109077
• Main Authors: Zhang, Zhiyong, Li, Dongsheng, Xu, Miaojun, Li, Bin
• Format: Journal Article
• Language: English
• Published: London Elsevier Ltd 01.03.2020; Elsevier BV
• Subjects: burning; calorimeters; chemical structure; Chemical synthesis; compression strength; Compressive strength; Cone calorimeters; Density; Expandable graphite; Flame retardants; Foaming; foams; Fourier transform infrared spectroscopy; Fourier transforms; Gas chromatography; gas chromatography-mass spectrometry; graphene; Graphite; Infrared radiation; Isocyanates; Mass spectrometry; Morphology; Nitrogen; NMR; Nuclear magnetic resonance; nuclear magnetic resonance spectroscopy; oxygen; phosphonates; Phosphorus; Phosphorus-nitrogen flame retardant; piperazine; Plastic foam; polyols; Polyurethane foam; polyurethanes; Rigid polyurethane foam; smoke; temperature; Thermogravimetric analysis; thermogravimetry; Rigid polyurethane foam; Expandable graphite; Phosphorus-nitrogen flame retardant
• ISSN: 0141-3910; 1873-2321
• DOI: 10.1016/j.polymdegradstab.2020.109077

A novel phosphorus and nitrogen containing flame retardant named 1,4-bis(Diethyl methylenephosphonate) piperazine (BDEMPP) was synthesized. The chemical structures of BDEMPP were determined by Fourier transform infrared spectrum (FTIR), nuclear magnetic resonance (NMR) and gas chromatography-mass spectrometry (GC-MS). The flame retardant rigid polyurethane foams (FR-RPUFs) were prepared by one-pot and free foaming with incorporating BDEMPP/expanded graphite (EG) with polyether polyol and polymethylene polyphenyl isocyanate. The limit oxygen index (LOI), vertical burning (UL94) and cone calorimeter (CONE) test showed that the fire-retardant properties were improved due to the barrier effect of EG and residual char. With addition of 10 wt % EG and 15 wt % BDEMPP, RPUF/10EG/15BDEMPP passed UL94 V-0 with the LOI value of 25.7%. The thermogravimetric analysis (TGA) results revealed that the initial decompose temperature (T5%) of RPUF/10EG/15BDEMPP was decreased compared with pure RPUF. However, the yield of residual char was increased from 0.35% for pure RPUF to 30.52% for RPUF/10EG/15BDEMPP at 800 °C. EG and BDEMPP had a slight influence on density and compression strength. The density and compression strength of pure RPUF was 45.42 kg m−3 and 213 kPa. As for RPUF/10EG/15BDEMPP, the density and compression strength was 44.18 kg m−3 and 180 kPa. The morphology and composition of residual char were investigated. The results demonstrated that the intact, compact and thick residual char with abundant of phosphorus and nitrogen was formed to enhance the flame retardancy and smoke suppression. •A novel phosphorus and nitrogen containing flame retardant named BDEMPP was synthesized and characterized.•The flame retardancy of RPUF was significantly improved by incorporation with BDEMPP and EG.•.The formation of residual char of RPUF/10EG/15BDEMPP was greater promoted to improve flame resistance.•EG and BDEMPP had a slight influence on density and compression strength.