Controllable fabrication of zinc borate hierarchical nanostructure on brucite surface for enhanced mechanical properties and flame retardant behaviors.
A novel and efficient halogen-free composite flame retardant (CFR) consisting of a brucite core and a fine zinc borate [Zn6O(OH)(BO3)3] hierarchical nanostructure shell was designed and synthesized via a facile nanoengineering route. It had been demonstrated that this unique hybrid structure possessed a high BET specific surface area (65 m(2)/g) and could significantly enhance the interfacial interaction when mixing with ethylene-vinyl acetate (EVA). This improved the transfer of stress between CFR particles and EVA matrix and increased the viscosity of EVA/EVA blends, which was beneficial for droplet inhibition and char forming. The mechanical properties and flammability behaviors of the EVA/CFR blends had been compared with the EVA/physical mixture (PM, with the given proportion of brucite and Zn6O(OH)(BO3)3). The mechanical properties of EVA/CFR blends, especially the tensile strength (TS), presented a remarkable increase reaching at least a 20% increment. Meanwhile, with the same 45 wt % of fillers, the EVA/CFR formulation could achieve a limiting oxygen index (LOI) value of 33 (37.5 % higher than that of EVA/PM blends) and UL-94 V-0 rating. Moreover, the heat release rate (HRR), peak heat release rate (PHRR), total heat released (THR), smoke production rate (SPR) and mass loss rate (MLR) were considerably reduced, especially PHRR and SPR for EVA/CFR blends were reduced to 32%. According to this study, the design of fine structure might pave the way for the future development of halogen-free flame retardants combining both enhanced mechanical properties and excellent flame retardant behaviors.
The Effects of a Macromolecular Charring Agent with Gas Phase and Condense Phase Synergistic Flame Retardant Capability on the Properties of PP/IFR Composites
In order to improve the efficiency of intumescent flame retardants (IFRs), a novel macromolecular charring agent named poly(ethanediamine-1,3,5-triazine-p-4-amino-2,2,6,6-tetramethylpiperidine) (PETAT) with gas phase and condense phase synergistic flame-retardant capability was synthesized and subsequently dispersed into polypropylene (PP) in combination with ammonium polyphosphate (APP) via a melt blending method. The chemical structure of PETAT was investigated by Fourier transform infrared spectroscopy (FTIR), and 1H nuclear magnetic resonance (NMR) spectroscopy. Thermal properties of the PETAT and IFR systems were tested by thermogravimetric-derivative thermogravimetric analysis (TGA-DTG) and thermogravimetry–Fourier transform infrared spectroscopy (TG-FTIR). The mechanical properties, thermal stability, flame-retardant properties, water resistance, and structures of char residue in flame-retardant composites were characterized using tensile and flexural strength property tests, TGA, limiting oxygen index (LOI) values before and after soaking, underwritten laboratory-94 (UL-94) vertical burning test, cone calorimetric test (CCT), scanning electron microscopy with energy dispersive X-ray spectrometry (SEM-EDXS), and FTIR. The results indicated that PETAT was successfully synthesized, and when the ratio of APP to PETAT was 2:1 with 25 wt % loading, the novel IFR system could reduce the deterioration of tensile strength and enhance the flexural strength of composites. Meanwhile, the flame-retardant composite was able to pass the UL-94 V-0 rating with an LOI value of 30.3%, and the peak of heat release rate (PHRR), total heat release (THR), and material fire hazard values were considerably decreased compared with others. In addition, composites also exhibited excellent water resistance properties compared with traditional IFR composites. SEM-EDXS and FTIR analyses of the char residues, as well as TG-FTIR analyses of IFR were used to investigate the flame-retardant mechanism of the APP/PETAT IFR system. The results indicated that the efficient flame retardancy of PP/IFR composites could be attributed to the synergism of the free radical-quenching and char layer-protecting mechanisms in the gas phase and condense phase, respectively.
HPLC determination of chlorhexidine gluconate and p-chloroaniline in topical ointment.
A novel fast isocratic reversed-phase HPLC method for simultaneous determination of chlorhexidine and its degradation product p-chloroaniline was developed. Zorbax SB Phenyl column (75 mm x 4.6 mm, 3.5 microm) was used for the separation. Mobile phase composed of acetonitrile and buffer solution of 0.08 M sodium phosphate monobasic containing 5 ml of triethylamine (0.5%) and adjust with 85% phosphoric acid to pH 3.0 in ratio 35:65 (v/v) pumped isocratically at flow rate 0.6 ml min(-1) was used. UV detection was performed at 239 nm, the total analysis time was about 10 min. The method is suitable for practical routine analysis of topical ointment in the quality control laboratory.