Citation: Xin-xin Wang, Wen-tao He, Guo-min Xu, Li-juan Long, Wei-jiang Huang, Jie Yu. Synergistic Flame Retardancy of Amine-based Multi-walled Carbon Nanotubes/DOPO Derivatives and Its Effect on the Properties of Nylon 6[J]. Acta Polymerica Sinica, ;2019, 50(4): 419-428. doi: 10.11777/j.issn1000-3304.2018.18230 shu

Synergistic Flame Retardancy of Amine-based Multi-walled Carbon Nanotubes/DOPO Derivatives and Its Effect on the Properties of Nylon 6

Xin-xin Wang ¹ ,
Wen-tao He ^2,, ,
Guo-min Xu ^2,, ,
Li-juan Long ² ,
Wei-jiang Huang ^1,2 ,
Jie Yu ^1,2

1.
College of Materials and Metallurgy, Guizhou University, Guiyang 550025
2.
National Engineering Research Center for Compounding and Modification of Polymer Materials, Guiyang 550014

Corresponding author: Wen-tao He, wentaohe@aliyun.com Guo-min Xu, jenny2000820@sina.com
Received Date: 22 November 2018
Revised Date: 18 January 2019
Available Online: 26 February 2019

A novel DOPO derivative (DIDOPO) is incorporated together with amine-based multi-walled carbon nanotubes (MWCNTs) into PA6 by melt blending. Mechanical properties, thermal stability, crystallinity, and combustion properties are measured using universal testing machine, thermogravimetric analyzer, differential scanning calorimeter, and cone calorimeter, respectively. After combustion, the morphology of char layer is further observed by a scanning electron microscope. The results show that MWCNTs-incorporated flame-retardant nanocomposites exhibit a tensile strength that is 55% higher than that of the PA6/DIDOPO composites. From the TG and DTG curves, it can be seen that the T_5wt% of PA6 composites increased slightly and the maximum weight loss rate temperature (T_max) gradually improved after adding MWCNTs, indicating that the addition of MWCNTs delays the process of thermal degradation of the PA6 composites. With the incorporation of MWCNTs, the amount of residual carbon is also increased. From the non-isothermal crystallization curve, it can be seen that the crystallization initial temperature (T_onset) and crystallization peak temperature (T_c) of the PA6 composites are significantly improved with the addition of MWCNTs. However, the crystallinity is lower due to the heterogeneous nucleation of the MWCNTs. From UL-94 datas, the combustion time (t₁ + t₂) is increased with the incorporation of MWCNTs into PA6/DIDOPO composites, which results in a V-1 level in the UL-94 test and a slightly increased LOI value. This phenomenon can be attributed to an increment in melt viscosity and a decrement in flow properties. Combined with the curves of effective combustion heat, total smoke release and CO release rate, it can be concluded that the synergistic effect between MWCNTs and DIDOPO weakens the thermal degradation process of the PA6 composites, thus increasing the incomplete combustion and reducing the complete combustion of the PA6 composites, which is beneficial to the flame retardance of the materials. Addition of 2 wt% MWCNTs results in a peak heat release rate (PHRR) of 367.28 kW/m², which corresponds to a 58.9% lower rate than that of pure PA6, as revealed by cone calorimetry. Based on SEM and Raman, a continuous and compact char layer is observed upon addition of MWCNTs, which is ascribed to a synergistic effect between MWCNTs and DIDOPO.
- Amine-based multi-walled carbon nanotubes,
- DOPO derivatives,
- Nylon 6,
- Thermal stability,
- Synergistic flame retardant
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