A Novel Organophosphorus Hybrid with Excellent Thermal Stability: Core-Shell Structure, Hybridization Mechanism, and Application in Flame Retarding Semi-Aromatic Polyamide.
An organophosphorous hybrid (BM@Al-PPi) with unique core-shell structure was prepared through hybridization reaction between boehmite (BM) as the inorganic substrate and phenylphosphinic acid (PPiA) as the organic modifier. Fourier transform infrared spectra (FTIR), solid state (31)P and (27)Al magic angle spinning nuclear magnetic resonance, X-ray diffraction, and element analysis were used to investigate the chemical structure of the hybrids, where the microrod-like core was confirmed as Al-PPi aggregates generated from the reaction between BM and PPiA, and those irregular nanoparticles in the shell belonged to residual BM. Compared with the traditional dissolution-precipitation process, a novel analogous suspension reaction mode was proposed to explain the hybridization process and the resulting product. Scanning electronic microscopy further proved the core-shell structure of the hybrids. BM exhibited much higher initial decomposition temperature than that of Al-PPi; therefore, the hybrid showed better thermal stability than Al-PPi, and it met the processing temperature of semi-aromatic polyamide (HTN, for instance) as an additive-type flame retardant. Limiting oxygen index and cone calorimetric analysis suggested the excellent flame-retardant performance and smoke suppressing activity by adding the resulting hybrid into HTN.
X-Ray study of zinc(II) di-n-alkylphosphinate copolymers
The mixed-ligand species Zn[(R12PO2)2 – 2x(R22PO2)2x](R1= Bun; R2= n-C6H13 or n-C10H21) are linear coordination copolymers with a random distribution of two different bridging phosphinate groups along the molecular chains. Single crystals of the copolymer {Zn[Bun2PO2(n-C6H13)2PO2]}n are disordered. A three-dimensional X-ray analysis has been attempted. The crystals contain chains characterised by a backbone structure with alternate single and triple bridging phosphinate groups between tetrahedral metal atoms. The structural features common to those of the β-form of zinc(II) di-n-butylphosphinate polymer are discussed.
Flame retardation of glass-fibre-reinforced polyamide 6 by a novel metal salt of alkylphosphinic acid
Abstract Aluminum salts of phosphinic acid mixture of diisobutylphosphinic acid and monoisobutylphosphinic acid (HPA-2TBA-Al) and glass fibres were compounded with polyamide 6 to prepare a series of flame retardant GF/PA6 composites via melt blending. The flame retardance and burning behaviors of the composites were investigated by limiting oxygen index (LOI), vertical burning test (UL-94), and Cone calorimeter test. The thermal properties and decomposition kinetics were investigated by thermogravimetric analysis (TGA) under N 2 atmosphere. Addition of HPA-2TBA-Al results in an increased LOI value, a UL-94 V-0 rating together with a decrease in both the values of PHRR and THR in Cone calorimetric analysis. Visual observations and scanning electronic microscopy (SEM) after flame retardant tests confirmed the char-formation which acts as a fire barrier in condense phase. Analysis of cone calorimeter data indicates that gas phase flame retardant mechanism exists in the GFPA6/HPA-2TBA-Al system.