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Synthesis of a novel aluminum salt of nitrogen-containing alkylphosphinate with high char formation to flame retard acrylonitrile –butadiene–styrene

Citation

Liu, Xueqing; Yang, Xue; wang, Hao; Liu, Jiyan (2020), Synthesis of a novel aluminum salt of nitrogen-containing alkylphosphinate with high char formation to flame retard acrylonitrile –butadiene–styrene, Dryad, Dataset, https://doi.org/10.5061/dryad.j9kd51c92

Abstract

A novel nitrogen-containing alkylphosphinate salt----aluminum β-(p-nitrobenzamide) ethyl methyl phosphinate (AlNP) was synthesized and used to flame retard acrylonitrile-butadiene-styrene copolymer (ABS). The Fourier transform infrared spectrometry, 1H, 13C and 31P nuclear magnetic resonance and X-ray fluorescent spectroscopy (XRF) were applied to characterize the structure and composition of products. The flame retardancy performance, thermal properties and mechanical strength of the ABS/AlNP with respect to AlNP loading were investigated. AlNP was stable before 330 oC and decomposed very slowly with residues high up to 56.1 % at 700 oC. Adding 25-30 wt% of AlNP alone can make ABS to pass V0 rating in the vertical burning tests (UL 94). The results according to the micro combustion calorimeter, thermogravimetric analysis showed that AlNP can depress the heating release and retard the thermal degradation of the ABS. Scanning electron microscopy observation for the residues from LOI test indicated that AlNP formed the condensed and tough residues layer during combustion; XRF analysis showed that the residues contained phosphorus and aluminum element and nitrogen element was not detected. The compact phosphorus/aluminium-rich substance acted as a barrier to enhance flame-retardant properties of the ABS.

Methods

  FTIR measurement was carried out using a Tensor 27 Bruker infrared spectrometer (Bruker, German) and operated at 4 cm-1 resolution.

The X-ray fluorescent spectroscopy (XRF) analysis of the sample was done on pressed powder pellet of 4 cm in diameter. The operation was performed on a ZSX Primus II (Rigaku, Japan) XRF spectrometer.

Thermogravimetric (TG) measurement was performed with TSDT Q600 (TA, USA) under N2 atmosphere   from 30 oC to 700 oC at heating rate of 20 oC min-1, using alumina crucibles and sample mass of about 9-10 mg.     

 Micro combustion calorimetric measurement (MCC) was performed with a MCC-2 instrument (Govmark, USA). The powder sample (about 7 mgwas heated from 40 oC to 700 oC in an aluminum crucible with heating rate 1 oC s-1. The heating atmosphere is a mixture of N2 (flow rate 80 ml min-1) and O2 (flow rate 20 ml min-1).

The glass transition temperature (Tg) was investigated with a Q-20 differential scanning calorimeter (DSC, TA, USA). The measurement was carried under N2 atmosphere (flow rate 50 ml min-1). The sample of 6-8 mg was used and heated from 30 oC to 250 oC at temperature rate of 10 oC min-1.

 

Usage Notes

No missing values

Funding

National Natural Science Foundation of China, Award: No.51303209

National Basic Research Program of China (973 Program), Award: No.2016YFB0401505

Key Scientific and Technological Project of Wuhan City, Award: No.2018010401011279

Key Scientific and Technological Project of Wuhan City, Award: No.2018010401011279