Synthesis of a novel, multifunctional inorganic curing agent and its effect on the flame-retardant and mechanical properties of intrinsically flame retardant epoxy resin

2018 ◽  
Vol 135 (29) ◽  
pp. 46410 ◽  
Author(s):  
Xing Guo ◽  
Hongsen Wang ◽  
Delong Ma ◽  
Jinnan He ◽  
Ziqiang Lei
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.


2015 ◽  
Vol 44 (1) ◽  
pp. 19-25
Author(s):  
T. Maity ◽  
B.C. Samanta

Purpose – The purpose of this paper was to check effectiveness of amine functional chloroaniline acetaldehyde condensate (AFCAC) as a new curing agent for diglycidyl ether of bisphenol A (DGEBA) resin. For this purpose, first AFCAC was synthesised, characterised and then curing reaction was carried out. Design/methodology/approach – Equimolecular mixture of AFCAC and DGEBA was subjected to curing reaction, and the reaction was followed by differential scanning calorimetry (DSC) analysis. The kinetic studies of this curing reaction were also carried out from those DSC exotherms. The mechanical properties, dynamic mechanical analysis (DMA) and thermogravimetric analysis (TGA) of cured epoxy were also reported. Findings – DSC results reflected the effective first order curing reaction of AFCAC with epoxy resin. Mechanical properties reflected appreciable rigidity of AFCAC cured epoxy matrix and TGA showed that the cured epoxy networks were thermally stable up to around 297°C. Research limitations/implications – The curing agent AFCAC was synthesised by using chloroaniline and acetaldehyde in acid medium. There are some limitations for this procedure. The synthetic procedure is pH dependent. So reaction cannot be done at any pH value. The reaction must also be carried out at room temperature without any heating. To obtain low molecular weight curing agent, chloroaniline and acetaldehyde cannot be taken in equimolecular ratio because the equimolecular mixture of them produces high molecular weight condensate. This was shown in our previous publication. Some implications are also there. By changing amine and aldehyde other curing agents could be synthesised and the curing efficiency of those for epoxy resin could also be studied. Originality/value – Experimental results revealed the greater suitability of AFCAC as curing agent for DGEBA resin and novelty of AFCAC cured matrix in the field of protective coating, casting, adhesives, etc.


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

Polymers ◽  
2020 ◽  
Vol 12 (10) ◽  
pp. 2349
Author(s):  
Woranan Netkueakul ◽  
Beatrice Fischer ◽  
Christian Walder ◽  
Frank Nüesch ◽  
Marcel Rees ◽  
...  

The effects of combining 0.1–5 wt % graphene nanoplatelet (GNP) and 3–30 wt % phosphorous flame retardant, 9,10- dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) as fillers in epoxy polymer on the mechanical, flame retardancy, and electrical properties of the epoxy nanocomposites was investigated. GNP was homogeneously dispersed into the epoxy matrix using a solvent-free three-roll milling process, while DOPO was incorporated into the epoxy resin by mechanical stirring at elevated temperature. The incorporation of DOPO reduced the crosslinking density of the epoxy resin. When using polyetheramine as a hardener, the structural rigidity effect of DOPO overshadowed the crosslinking effect and governed the flexural moduli of epoxy/DOPO resins. The flexural moduli of the nanocomposites were improved by adding GNP up to 5 wt % and DOPO up to 30 wt %, whereas the flexural strengths deteriorated when the GNP and DOPO loading were higher than 1 wt % and 10 wt %, respectively. Limited by the adverse effects on mechanical property, the loading combinations of GNP and DOPO within the range of 0–1 wt % and 0–10 wt %, respectively, in epoxy resin were further studied. Flame retardancy index (FRI), which depended on three parameters obtained from cone calorimetry, was considered to evaluate the flame retardancy of the epoxy composites. DOPO showed better performance than GNP as the flame retardant additive, while combining DOPO and GNP could further improve FRI to some extent. With the combination of 0.5 wt % GNP and 10 wt % DOPO, improvement in both mechanical properties and flame retardant efficiency of the nanocomposite was observed. Such a combination did not affect the electrical conductivity of the nanocomposites since the percolation threshold was at 1.6 wt % GNP. Our results enhance the understanding of the structure–property relationship of additive-filled epoxy resin composites and serve as a property constraining guidance for the composite manufacturing.


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.


2017 ◽  
Vol 29 (1) ◽  
pp. 603-611 ◽  
Author(s):  
Ting Chen ◽  
Xianming Chen ◽  
Meijie Wang ◽  
Peixin Hou ◽  
Cao Jie ◽  
...  

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