A novel high phosphorus‐efficiency phosphaphenanthrene curing agent for fabricating flame retardant and toughened epoxy thermoset

Author(s):  
Zhongying Yao ◽  
Yong Qiu ◽  
Lijun Qian ◽  
Bo Xu
Polymers ◽  
2022 ◽  
Vol 14 (2) ◽  
pp. 245
Author(s):  
Yong Sun ◽  
Yongli Peng ◽  
Yajiao Zhang

In this work, a flame retardant curing agent (DOPO-MAC) composed of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide DOPO and methyl acrylamide (MAC) was synthesized successfully, and the structure of the compound was characterized by FT-IR and 1H-NMR. The non-isothermal kinetics of the epoxy resin/DOPO-MAC system with 1% phosphorus was studied by non-isothermal DSC method. The activation energy of the reaction (Ea), about 46 kJ/mol, was calculated by Kissinger and Ozawa method, indicating that the curing reaction was easy to carry out. The flame retardancy of the epoxy resin system was analyzed by vertical combustion test (UL94) and limiting oxygen index (LOI) test. The results showed that epoxy resin (EP) with 1% phosphorus successfully passed a UL-94 V-0 rating, and the LOI value increased along with the increasing of phosphorus content. It confirmed that DOPO-MAC possessed excellent flame retardance and higher curing reactivity. Moreover, the thermal stability of EP materials was also investigated by TGA. With the DOPO-MAC added, the residual mass of EP materials increased remarkably although the initial decomposition temperature decreased slightly.


e-Polymers ◽  
2019 ◽  
Vol 19 (1) ◽  
pp. 545-554 ◽  
Author(s):  
Anxin Li ◽  
Pingli Mao ◽  
Bing Liang

AbstractIn order to improve the compatibility of flame retardant and epoxy resin, a phosphorus nitrogen flame retardant curing agent poly(p-xylylenediamine spirocyclic pentaerythritol bisphosphonate) (PPXSPB) was synthesized. FTIR, 1HNMR, and mass spectroscopy were used to identify the chemical structure of PPXSPB. Epoxy resin (E-44) and PPXSPB as the raw material, a series of thermosetting systems were prepared. The effects of PPXSPB on flame retardancy, water resistance, thermal degradation behavior, mechanical properties and the adhesive strength of EP/PPXSPB thermosets were investigated. The results show that with the increase of phosphorus content, the oxygen index and carbon residue of the system both increased significantly, and the heat release rate gradually decreased, which is of great significance in delaying the occurrence of fire. When the phosphorus content is 3.24% in EP/PPXSPB thermosets, EP-2 can successfully pass the UL94 V-0 flammability rating, the LOI value of EP-2 can reach 31.4%, the impact strength and tensile strength was 6.58 kJ/m2 and 47.10 MPa respectively, and the adhesive strength was 13.79 MPa, the system presents a good overall performance.


2019 ◽  
Vol 163 ◽  
pp. 100-109 ◽  
Author(s):  
Siqi Huo ◽  
Zhitian Liu ◽  
Chuan Li ◽  
Xiaolei Wang ◽  
Haopeng Cai ◽  
...  

2016 ◽  
Vol 56 (4) ◽  
pp. 441-447 ◽  
Author(s):  
Cong Xie ◽  
Jifu Du ◽  
Zhen Dong ◽  
Shaofa Sun ◽  
Long Zhao ◽  
...  

2015 ◽  
Vol 7 (32) ◽  
pp. 17919-17928 ◽  
Author(s):  
Yi Tan ◽  
Zhu-Bao Shao ◽  
Xue-Fang Chen ◽  
Jia-Wei Long ◽  
Li Chen ◽  
...  

2017 ◽  
Vol 30 (10) ◽  
pp. 1229-1239 ◽  
Author(s):  
Shan Huang ◽  
Xiao Hou ◽  
Jiaojiao Li ◽  
Xiujuan Tian ◽  
Qing Yu ◽  
...  

A phosphorous/nitrogen-containing diphenylphosphine oxide (DPO) derivative (DPO-SS) was designed and synthesized via a two-step reaction of 4,4′-diaminodiphenylsulfone, 2-hydroxy-benzaldehyde, and DPO. The structure of DPO-SS was confirmed by Fourier transform infrared spectroscopy (FTIR), 1H and 31P nuclear magnetic resonance (NMR) spectroscopy, and mass spectrometry (MS). DPO-SS was used as a flame retardant and curing agent for copolymerizing with diglycidyl ether of bisphenol-A. Thermal and flame-retardant properties of the obtained flame-retardant epoxy resin (F-EP) were investigated by thermogravimetric analysis, dynamic thermomechanical analysis, limited oxygen index (LOI) measurement, vertical burning test (UL-94), and cone calorimeter test. Results indicated that all F-EP samples exhibited excellent thermal stability and flame-retardant property. Especially for F-EP with P content of 0.7 wt% (denoted as EP/P-0.7), it achieved high LOI values (32.4%) and UL-94 V-0 rating. Compared with pure EP, all F-EP samples showed lower heat release rate, total heat release, total smoke produce, and little Tg fluctuation. In order to study the flame-retardant mechanism, the char residues were investigated by FTIR, scanning electron microscopy, and energy-dispersive spectrometer analysis. The results manifested that DPO-SS acted as flame retardant in both gas phase and condensed phase. Water absorption properties of pure EP and F-EP were also compared through immersion experiments. Results showed that EP/P-0.7 sample had apparently lower water absorptivity than pure EP.


1991 ◽  
Vol 27 (1) ◽  
pp. 29-30
Author(s):  
A.J. Taylor ◽  
M. Ballard

1999 ◽  
Vol 19 (3) ◽  
pp. 151-160 ◽  
Author(s):  
A.D. La Rosa ◽  
S. Failla ◽  
P. Finocchiaro ◽  
A. Recca ◽  
V. Siracusa ◽  
...  

Abstract A new ortho-hydroxy-aryl-phosphonate additive was used to improve the flame resistance of an epoxy/anhydride system. Thermal, rheological, L.O.l. and SEM experiments were carried out to show that the P-additive acts not only as a flame retardant but also as a curing agent.


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