Flame-retardant halogen-free polymers using phosphorylated hexaglycidyl epoxy resin

2017 ◽  
Vol 30 (2) ◽  
pp. 202-210 ◽  
Author(s):  
Rasool Kheyrabadi ◽  
Hossein Rahmani ◽  
S Heydar Mahmoudi Najafi
Keyword(s):  
Flame Retardant ◽  
Epoxy Resin ◽  
Phosphine Oxide ◽  
Flame Retardancy ◽  
High Performance ◽  
Liquid Chromatography Mass Spectrometry ◽  
Scanning Calorimetry ◽  
Epoxy Monomer ◽  
Ul 94 ◽  
Halogen Free

Flame-retardant halogen-free epoxy resin, containing phosphorus and nitrogen atoms in the main chain, was synthesized through the curing of tris(3-(bis(oxiran-2-ylmethyl)amino)phenyl)phosphine oxide (HGE, hexaglycidyl epoxy monomer), starting from tris(3-aminophenyl) phosphine oxide (TAPO) and epichlorohydrin. The molecular structure of HGE with molecular weight 660 was confirmed using Fourier transform infrared, nuclear magnetic resonance, and liquid chromatography–mass spectrometry techniques. Epoxy equivalent weight determined by titration method was 120. The thermal curing behavior of the HGE/TAPO was investigated by differential scanning calorimetry. An intense exotherm due to curing reaction was observed in the temperature range from 123°C to 215°C. The HGE cured with TAPO, 4,4′-diaminodiphenylsulfone (DDS), and 1,5-diaminonaphthalene (DAN) and the thermal behaviors were studied by thermogravimetric analysis. The flame retardancy properties of the HGE/TAPO, DDS, and DAN were evaluated by vertical burning test (UL-94 V). The high performance cured epoxy resins showed high thermal stability and UL-94 V-0 flame retardancy rating.

scholarly journals Recent Developments in the Flame-Retardant System of Epoxy Resin

Materials ◽  
2020 ◽  
Vol 13 (9) ◽  
pp. 2145 ◽  
Author(s):  
Quanyi Liu ◽  
Donghui Wang ◽  
Zekun Li ◽  
Zhifa Li ◽  
Xiaoliang Peng ◽  
...  
Keyword(s):  
Thermal Stability ◽  
Heat Resistance ◽  
Flame Retardant ◽  
Epoxy Resin ◽  
Flame Retardancy ◽  
High Performance ◽  
Flame Retardants ◽  
Great Progress ◽  
Recent Developments ◽  
Halogen Free

With the increasing emphasis on environmental protection, the development of flame retardants for epoxy resin (EP) has tended to be non-toxic, efficient, multifunctional and systematic. Currently reported flame retardants have been capable of providing flame retardancy, heat resistance and thermal stability to EP. However, many aspects still need to be further improved. This paper reviews the development of EPs in halogen-free flame retardants, focusing on phosphorus flame retardants, carbon-based materials, silicon flame retardants, inorganic nanofillers, and metal-containing compounds. These flame retardants can be used on their own or in combination to achieve the desired results. The effects of these flame retardants on the thermal stability and flame retardancy of EPs were discussed. Despite the great progress on flame retardants for EP in recent years, further improvement of EP is needed to obtain numerous eco-friendly high-performance materials.

Synthesis of a phosphorus–nitrogen-containing flame retardant and its application in epoxy resin

2018 ◽  
Vol 31 (2) ◽  
pp. 186-196 ◽  
Author(s):  
Shuang Yang ◽  
Yefa Hu ◽  
Qiaoxin Zhang
Keyword(s):  
Heat Release ◽  
Flame Retardant ◽  
Epoxy Resin ◽  
Heat Release Rate ◽  
Flame Retardancy ◽  
Release Rate ◽  
Epoxy Resins ◽  
Proton Nuclear Magnetic Resonance ◽  
Scanning Calorimetry ◽  
Cone Calorimeter Test

In this article, a phosphorus–nitrogen-containing flame retardant (DOPO-T) was successfully synthesized by nucleophilic substitution reaction between 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and cyanuric chloride. The chemical structure of DOPO-T was characterized by Fourier transform infrared spectroscopy, proton nuclear magnetic resonance (NMR) and phosphorous-31 NMR, and elemental analysis. DOPO-T was then blended with diglycidyl ether of bisphenol-A to prepare flame-retardant epoxy resins. Thermal properties, flame retardancy, and combustion behavior of the cured epoxy resins were evaluated by differential scanning calorimetry, thermogravimetric analysis, limited oxygen index (LOI) measurement, UL94 vertical burning test, and cone calorimeter test. The results indicated that the glass transition temperature ( Tg) and temperature at 5% weight loss of epoxy resin (EP)/DOPO-T thermosets were gradually decreased with the increasing content of DOPO-T. DOPO-T catalyzed the decomposition of EP matrix in advance. The flame-retardant performance of EP thermosets was significantly enhanced with the addition of DOPO-T. EP/DOPO-T-0.9 sample had an LOI value of 36.2% and achieved UL94 V-1 rating. In addition, the average of heat release rate, peak of heat release rate, average of effective heat of combustion, and total heat release (THR) of EP/DOPO-T-0.9 sample were decreased by 32%, 48%, 23%, and 31%, respectively, compared with the neat EP sample. Impressively, EP/DOPO-T thermosets acquired excellent flame retardancy under low loading of flame retardant.

scholarly journals Preparation of Intercalated Organic Montmorillonite DOPO-MMT by Melting Method and Its Effect on Flame Retardancy to Epoxy Resin

Polymers ◽  
2021 ◽  
Vol 13 (20) ◽  
pp. 3496
Author(s):  
Junming Geng ◽  
Jianyu Qin ◽  
Jiyu He
Keyword(s):  
Electron Microscopy ◽  
Flame Retardant ◽  
Epoxy Resin ◽  
Flame Retardancy ◽  
Flame Retardants ◽  
Characterization Methods ◽  
Melting Method ◽  
Organic Montmorillonite ◽  
Ul 94 ◽  
Flame Retardant Properties

An intercalated organic montmorillonite DOPO-MMT was prepared through the melting method using 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) as a modifier. Epoxy resin (EP) composites were prepared with DOPO-MMT, DOPO, MMT, and the physical mixtures of DOPO+MMT as flame retardants. The microstructure of the flame retardants and EP samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The flame retardant properties, thermal stability, and residual char structure of the EPs were studied by the limited oxygen index (LOI) test, the UL-94 vertical burning test, thermogravimetric analysis (TGA), the differential scanning calorimeter (DSC) test, the cone calorimeter (CONE) test as well as other characterization methods. The results showed that the intercalated organic montmorillonite DOPO-MMT can be successfully prepared by the melting method and that the MMT is evenly dispersed in the EP/DOPO-MMT composite in the form of nanosheets. The EP/DOPO-MMT nanocomposites showed the optimal flame retardancy (LOI, UL-94, PHRR, etc.) among the EPs with DOPO, MMT, and the physical mixture of DOPO+MMT. The flame-retardant grade of the material reached V-0.

scholarly journals PREPARATION OF IRON- REDUCED GRAPHENE OXIDE/ EPOXY RESIN COMPOSITE AND ITS FLAME RETARDANCY AND THERMAL STABILITY

10.6036/10327 ◽  
2022 ◽  
Vol 97 (1) ◽  
pp. 98-103
Author(s):  
XIAN WANG ◽  
JINLONG ZHUO ◽  
TIANQING XING ◽  
Xingran Wang
Keyword(s):  
Thermal Stability ◽  
Graphene Oxide ◽  
Flame Retardant ◽  
Epoxy Resin ◽  
Iron Powder ◽  
Flame Retardancy ◽  
Limiting Oxygen Index ◽  
Cone Calorimeter Test ◽  
Industrial Manufacture ◽  
Ul 94

In order to reduce flammability, smoke release and enhance thermal stability of epoxy resin (EP), iron powder is mixed with graphene oxide/ epoxy resin (GO/EP) composite by mechanical blending. The combustion performance of composite material is investigated through limiting oxygen index (LOI), Underwriters Laboratory (UL)-94 test, and cone calorimeter test (CCT). Thermogravimetric-Fourier transform infrared spectroscopy (TG-FTIR) and scanning electron microscope (SEM) are also used to explore the mechanism of flame retardancy and smoke suppression. Results show that, with the addition of 0.5% mass fraction of GO and the corresponding iron powder combination (EP3 sample), the LOI value can achieve 32.5% while reaching the UL-94 V0 rating. Compare with EP0, the peaks of heat release rate, smoke production rate, and smoke factor values of EP3 are decreased by 42%, 60%, and 50%, respectively. The char and TG-FTIR data of EP3 reveal that it has a more compact structure, good thermal stability, and produce fewer toxic gases and smoke. Reduction of GO could inhibit the degradation of EP, and iron catalyzes the formation of carbonaceous char on the surface. Thus, the thermal stability and flame retardancy of EP are improved significantly. This study provides a suitable way to prepare graphene/EP composites that contain iron catalyst and can be extended to the industrial manufacture of flame retardant polymer composites. Keywords: iron powder; epoxy resin; graphene oxide; flame retardant; thermal stability

Flame Retardancy of Lanthanum Phosphinate in Combination with Intumescen Flame-Retardant in Polypropylene

2012 ◽  
Vol 490-495 ◽  
pp. 3366-3369 ◽  
Author(s):  
Cong Liu
Keyword(s):  
Thermogravimetric Analysis ◽  
Flame Retardant ◽  
Flame Retardancy ◽  
Oxygen Index ◽  
Intumescent Flame Retardant ◽  
Limiting Oxygen Index ◽  
Ul 94 ◽  
Halogen Free

The flame-retardant of Lanthanum phenylphosphinate(LaPi) was prepared and its combination with intumescent flame retardant (IFR) in polypropylene (PP) was analysed using thermogravimetric analysis (TGA), limiting oxygen index (LOI) and the UL-94 test. Compared with using IFR alone, using the combination of LaPi and IFR gained the better classification in the UL 94 test thanks to the combination of the different mechanisms. When 20 wt% loading of flame retardant of LaPi and IFR, a halogen-free V-0 PP material was achieved with a LOI of 31%.

scholarly journals Polycarbonate/Sulfonamide Composites with Ultralow Contents of Halogen-Free Flame Retardant and Desirable Compatibility

Materials ◽  
2020 ◽  
Vol 13 (17) ◽  
pp. 3656
Author(s):  
Hangfeng Yang ◽  
Hangbo Yue ◽  
Xi Zhao ◽  
Minzimo Song ◽  
Jianwei Guo ◽  
...  
Keyword(s):  
Flame Retardant ◽  
Flame Retardancy ◽  
Oxygen Index ◽  
Smoke Emission ◽  
Limiting Oxygen Index ◽  
Ul 94 ◽  
Flame Retardant Properties ◽  
Halogen Free ◽  
Sem Morphology ◽  
Limited Oxygen

A novel halogen-free flame retardant containing sulfonamide, 1,3,5,7-tetrakis (phenyl-4-sulfonamide) adamantane (FRSN) was synthesized and used for improving the flame retardancy of largely used polycarbonate (PC). The flame-retardant properties of the composites with incorporation of varied amounts of FRSN were analyzed by techniques including limited oxygen index, UL 94 vertical burning, and cone calorimeter tests. The new FR system with sulfur and nitrogen elements showed effective improvements in PC’s flame retardancy: the LOI value of the modified PC increased significantly, smoke emission suppressed, and UL 94 V-0 achieved. Typically, the composite with only 0.08 wt% of FRSN added (an ultralow content) can increase the limiting oxygen index (LOI) value to 33.7% and classified as UL 94 V-0 rating. Furthermore, the mechanical properties and SEM morphology indicated that the FRSN has very good compatibility with PC matrix, which, in turn, is beneficial to the property enhancement. Finally, the analysis of sample residues after burning tests showed that a high portion of char was formed, contributing to the PC burning protection. This synthesized flame retardant provides a new way of improving PC’s flame retardancy and its mechanical property.

Synthesis and Properties of Flame-Retardant Waterborne Emulsion Derived from O-Cresol Formaldehyde Epoxy Resin

2013 ◽  
Vol 652-654 ◽  
pp. 84-88
Author(s):  
Jian Xiong Wei ◽  
Gui Long Xu ◽  
Jian Hu ◽  
Jin Yang
Keyword(s):  
Acetic Acid ◽  
Flame Retardant ◽  
Epoxy Resin ◽  
Condensed Phase ◽  
Flame Retardancy ◽  
Phosphorus Content ◽  
Flame Retardant Property ◽  
Ul 94 ◽  
Waterborne Emulsion ◽  
Epoxy Emulsion

By modifying O-cresol Formaldehyde epoxy resin with DOPO and Diethanolamine, and then neutralized by acetic acid, phosphorous-containing epoxy emulsion with excellent flame retardancy can be obtained under strong agitation. Diethanolamine opening rate and neutralized degree to the formation of epoxy emulsion were optimized. The flame-retardant property of the cured phosphorous-containing epoxy resin was test by UL-94, LOI and TGA method. The result shows that when the opening rate of Diethanolamine is 25.0% and the neutralized degree is 95.0%, stable epoxy emulsion can be obtained. When phosphorus content of the epoxy resin was 3.0wt%, the LOI value of the resin can be reach to 39.2 and pass the UL-94 test，the 700°C char remaining is 30.0wt%. The result shows that the flame retardant mechanism of the phosphorous-containing epoxy resin is mainly through a condensed- phase mechanism.

scholarly journals Dual UV-Thermal Curing of Biobased Resorcinol Epoxy Resin-Diatomite Composites with Improved Acoustic Performance and Attractive Flame Retardancy Behavior

2021 ◽  
Vol 2 (1) ◽  
pp. 24-48
Author(s):  
Quoc-Bao Nguyen ◽  
Henri Vahabi ◽  
Agustín Rios de Anda ◽  
Davy-Louis Versace ◽  
Valérie Langlois ◽  
...  
Keyword(s):  
Heat Release ◽  
Flame Retardant ◽  
Epoxy Resin ◽  
Flame Retardancy ◽  
Sound Absorption ◽  
Flexural Modulus ◽  
Construction Materials ◽  
Acoustic Properties ◽  
Low Frequencies ◽  
Compacting Pressure

This study has developed novel fully bio-based resorcinol epoxy resin–diatomite composites by a green two-stage process based on the living character of the cationic polymerization. This process comprises the photoinitiation and subsequently the thermal dark curing, enabling the obtaining of thick and non-transparent epoxy-diatomite composites without any solvent and amine-based hardeners. The effects of the diatomite content and the compacting pressure on microstructural, thermal, mechanical, acoustic properties, as well as the flame behavior of such composites have been thoroughly investigated. Towards the development of sound absorbing and flame-retardant construction materials, a compromise among mechanical, acoustic and flame-retardant properties was considered. Consequently, the composite obtained with 50 wt.% diatomite and 3.9 MPa compacting pressure is considered the optimal composite in the present work. Such composite exhibits the enhanced flexural modulus of 2.9 MPa, a satisfying sound absorption performance at low frequencies with Modified Sound Absorption Average (MSAA) of 0.08 (for a sample thickness of only 5 mm), and an outstanding flame retardancy behavior with the peak of heat release rate (pHRR) of 109 W/g and the total heat release of 5 kJ/g in the pyrolysis combustion flow calorimeter (PCFC) analysis.

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