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Chinese Journal of Materials Research  2021, Vol. 35 Issue (12): 918-924    DOI: 10.11901/1005.3093.2021.393
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Synthesis of Carbon Nanosphere-Based Nitrogen-Phosphorus-Sulfur Compound Flame Retardant and Flame Retardancy of CNSs-H-D Reinforced Epoxy Resin
JI Yaming1, YANG Yaru1,2(), YAO Yongbo1,2, LI Jiaqian1, SHEN Xiaojun1,2, LIU Shuqiang3
1.School of Materials and Textile Engineering, Jiaxing University, Jiaxing 314001, China
2.Zhejiang Key Laboratory of Yarn Material Forming and Composite Processing Technology, Jiaxing 314001, China
3.School of Textile Engineering, Taiyuan University of Technology, Jinzhong 030600, China
Cite this article: 

JI Yaming, YANG Yaru, YAO Yongbo, LI Jiaqian, SHEN Xiaojun, LIU Shuqiang. Synthesis of Carbon Nanosphere-Based Nitrogen-Phosphorus-Sulfur Compound Flame Retardant and Flame Retardancy of CNSs-H-D Reinforced Epoxy Resin. Chinese Journal of Materials Research, 2021, 35(12): 918-924.

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Abstract  

Carbon nanosphere based nitrogen-phosphorus-sulfur composite flame retardant (CNSs-H-D) was synthesized with the desired carbon nanospheres (CNSs) as core, hexachlorocyclotriphosphazene (HCCP) as bridge and amino diphenyl sulfone (DDS) as grafting agent. The morphology and thermal stability of CNSs-H-D were characterized. Afterwards, the composite of CNSs-H-D reinforced epoxy resin (EP) (CNSs-H-D/EP) was made and its flame retardancy and the relevant mechanism were investigated. Results show that the synthesized CNSs-H-D displayed a spherical morphology with a mean diameter of 80 nm and excellent thermal stability. Specifically, the LOI of CNSs-H-D/EP increased from 20.0% (of pure EP) to 27.5% (with addition of 5%(mass fraction) CNSs-H-D/EP), thus its flame retardance reached grade V-2 and its peak value of heat-release rate and fire-risk index reduced by 16.8% and 42.2%, respectively. Moreover, CNSs-H-D could significantly improve the thermal stability and char formation of EP. The initial decomposition temperature and high-temperature char residue of CNSs-H-D/EP increased by 40℃ and 144.7% respectively, in comparison with the pure EP. Furthermore, the initial weight loss temperature of CNSs-H-D/EP was 190℃ higher than that of EP. With good compactness and continuity of char layer, the CNSs-H-D/EP exhibited a typical condensed phase flame-retardant mechanism, where the char residue was as high as 94.5% at 800℃.

Key words:  composite      nitrogen-phosphorus-sulfur compound flame retardant      carbon nanospheres      epoxy resin      flame retardant     
Received:  05 July 2021     
ZTFLH:  TB332  
Fund: Natural Science Foundation of Zhejiang Province(LQ21E030008);National College Student Innovation and Entrepreneurship Training Program(CD851920510);Student Research and Training (SRT) Project of Jiaxing University(CD8517203298);Open Project Program of Key Laboratory of Yarn Materials Forming and Composite Processing Technology of Zhejiang Province(MTC2020-09)
About author:  YANG Yaru, Tel:15235409642, E-mail: yyr0515@zjxu.edu.cn

URL: 

https://www.cjmr.org/EN/10.11901/1005.3093.2021.393     OR     https://www.cjmr.org/EN/Y2021/V35/I12/918

SamplesE-51/gCYDHD-593/gCNSs-H-D/g
EP-0100280
EP-110026.721.28
EP-210024.163.84
EP-310021.66.4
Table 1  Formula of flame-retardant EP composites
Fig.1  SEM and EDS images of CNSs (a) and CNSs-H-D (b)
Fig.2  Infrared spectra of DDS, HCCP (a) and CNSs, CNSs-H-D (b)
Fig.3  TG curves of CNSs and CNSs-H-D
Samples

LOI

/%

UL-94 vertical burning test
t1/t2/st3/sIgnitecottonRate
EP-020.0>30>60YesNR
EP-123.06.8/5.16.0YesV-2
EP-225.85.5/3.34.0YesV-2
EP-327.53.9/1.92.2YesV-2
Table 2  Vertical burning test results of LOI and UL-94
Fig.4  Curves of HRR (a) and THR (b)
SamplesEP-0EP-1EP-2EP-3
TTI / s27293839
pk-HRR / kW·m-21372.291203.011168.311146.12
THR / MJ·m-2262.45230.50227.45218.32
pk-HRR/TTI /kW·(m2·s)-150.8341.4830.7529.39
Table 3  Data of cone calorimeter test
Fig.5  TG (a) and DTG (b) curves of EP and CNSs-H-D/EP
Fig.6  SEM images of the char residues of EP (a , A) and CNSs-H-D/EP (b , B)
Fig.7  TG curves of the char residues
Fig.8  Infrared spectra of the char residues
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