scholarly journals The application of a phosphorus nitrogen flame retardant curing agent in epoxy resin

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.

2020 ◽  
Vol 15 ◽  
pp. 155892502090132
Author(s):  
Sang-Hoon Lee ◽  
Seung-Won Oh ◽  
Young-Hee Lee ◽  
Il-Jin Kim ◽  
Dong-Jin Lee ◽  
...  

To prepare flame-retardant epoxy resin, phosphorus compound containing di-hydroxyl group (10-(2,5-dihydroxyphenyl)-9,10-dihydro-9-oxa-10-phospha phenanthrene-10-oxide, DOPO-HQ) was reacted with uncured epoxy resin (diglycidyl ether of bisphenol A, YD-128) and then cured using a curing agent (dicyandiamide, DICY). This study focused on the effect of phosphorus compound/phosphorus content on physical properties and flame retardancy of cured epoxy resin. The thermal decomposition temperature of the cured epoxy resins (samples: P0, P1.5, P2.0, and P2.5, the number represents the wt% of phosphorus) increased with increasing the content of phosphorus compound/phosphorus (0/0, 19.8/1.5, 27.8/2.0, and 36.8/2.5 wt%) based on epoxy resin. The impact strength of the cured epoxy resin increased significantly with increasing phosphorus compound content. As the phosphorus compound/phosphorus content increased from 0/0 to 36.8/2.5 wt%, the glass transition temperature (the peak temperature of loss modulus curve) increased from 135.2°C to 142.0°C. In addition, as the content of phosphorous compound increased, the storage modulus remained almost constant up to higher temperature. The limiting oxygen index value of cured epoxy resin increased from 21.1% to 30.0% with increasing phosphorus compound/phosphorus content from 0/0 to 36.8/2.5 wt%. The UL 94 V test result showed that no rating for phosphorus compounds less than 19.8 wt% and V-1 for 27.8 wt%. However, when the phosphorus compound was 36.8 wt%, the V-0 level indicating complete flame retardancy was obtained. In conclusion, the incorporation of phosphorus compounds into the epoxy chain resulted in improved properties such as impact strength and heat resistance, as well as a significant increase in flame retardancy.


2011 ◽  
Vol 399-401 ◽  
pp. 597-601
Author(s):  
Hai Da Liao ◽  
Wei Ping Zhang ◽  
Xiao Ming Sun ◽  
Jin Fu Qin ◽  
Yong Duo Hang

Abstract: Using laboratory-made nano-scale r–AlOOH as nanophase raw material, the compounding method characterized by direct solution-blending was adopted to prepare epoxy resin/AlOOH nano-composite material; the influences of various factors, such as the dispersion characteristics of nano-scale AlOOH and its content in composite material, on mechanical and flame retardant properties of composite material were studied. The result indicated that the epoxy resin/AlOOH nano-composite material, compared with the ordinary Al(OH)3/epoxy resin composite material, possessed excellent mechanical and flame retardant properties. When the content of AlOOH was 10%, the tensile strength and the breaking elongation rate of composite material was increased by 189% and 468%, respectively. When the mass ratio of AlOOH/epoxy resin was 70/100, the impact strength was increased by 59%; after it decreased to about 60/100, the vertical combustion reached the level of V-0.


Materials ◽  
2021 ◽  
Vol 14 (9) ◽  
pp. 2205
Author(s):  
Qian Li ◽  
Yujie Li ◽  
Yifan Chen ◽  
Qiang Wu ◽  
Siqun Wang

A novel liquid phosphorous-containing flame retardant anhydride (LPFA) with low viscosity was synthesized from 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and methyl tetrahydrophthalic anhydride (MeTHPA) and further cured with bisphenol-A epoxy resin E-51 for the preparation of the flame retardant epoxy resins. Both Fourier transform infrared spectroscopy (FT-IR), mass spectrometry (MS) and nuclear magnetic resonance (NMR) measurements revealed the successful incorporation of DOPO on the molecular chains of MeTHPA through chemical reaction. The oxygen index analysis showed that the LPFA-cured epoxy resin exhibited excellent flame retardant performance, and the corresponding limiting oxygen index (LOI) value could reach 31.2%. The UL-94V-0 rating was achieved for the flame retardant epoxy resin with the phosphorus content of 2.7%. With the addition of LPFA, the impact strength of the cured epoxy resins remained almost unchanged, but the flexural strength gradually increased. Meanwhile, all the epoxy resins showed good thermal stability. The glass transition temperature (Tg) and thermal decomposition temperature (Td) of epoxy resin cured by LPFA decreased slightly compared with that of MeTHPA-cured epoxy resin. Based on such excellent flame retardancy, low viscosity at room temperature and ease of use, LPFA showed potential as an appropriate curing agent in the field of electrical insulation materials.


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.


2013 ◽  
Vol 401-403 ◽  
pp. 713-716
Author(s):  
Cheng Fang ◽  
Dong Bo Guan ◽  
Wei Guo Yao ◽  
Shou Jun Wang ◽  
Hui An

The epoxy resin was modified with the mixture of α,ω-dihydroxy poly-(3,3,3-trifluoropropyl) siloxane (PTFPMS), KH560 and stannous octoate. KH560 can react with PTFPMS and also epoxy resin curing agent. The two reactions were characterized by FI-IR. The modified epoxy resin was characterized by FI-IR. The result showed that fluorine-containing silicone had been successfully introduced into the epoxy system. The mechanical and thermal properties of the modified epoxy resin were analyzed. The results showed that with the increase of PTFPMS the impact strength of epoxy resin increased, hardness and bending strength correspondingly reduced, slight decrease in the glass transition temperature.


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

2015 ◽  
Vol 744-746 ◽  
pp. 1463-1466
Author(s):  
Xi Wang

This paper presents the synthesis of a new type of flexible epoxy curing agent and an approach to improve the toughness of epoxy resin by curing without reducing the strength and modulus of the resin-cured material. The results show that the degree of toughness reaches maximum values when the flexible curing agent is applied at weight percentages (wt.%) between 10% and 15%. When the amount of flexible curing agent added to epoxy resin weight is 10wt.%, the impact toughness and fracture toughness increases by 33.3% and 96.3%, respectively, compared with the pure epoxy resin. When the amount of flexible curing agent added to epoxy is 10wt.%, the resulting impact thoughness of the material is 19.5 kJ•m-2 at-50°C, the impact toughness of pure epoxy resin is only 7.96 kJ•m-2.


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

2014 ◽  
Vol 926-930 ◽  
pp. 198-201
Author(s):  
Li Ying Guo ◽  
Jin Lin Liu ◽  
Peng Cheng Huang ◽  
Jun Hai He ◽  
Shi Yang Bai ◽  
...  

Polyether imidazole ionic liquid (PIIL) was blended with general-purpose epoxy resin (EP). PIIL/EP was cured by ethylenediamine curing agent. The structure of PIIL/EP was determined by FTIR. The effect of the content of PIIL on the impact strength of EP was studied. The toughness of epoxy resin could be significantly improved by PIIL. The impact strength of the modified EP was improved with the increase of PIIL and leveled off when the content of PIIL was more than 45%, and the modified EP showed rubber elasticity obviously.


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.


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