Synthesis and properties of a new halogen-free flame retardant for polyethylene

2018 ◽  
Vol 47 (3) ◽  
pp. 208-215 ◽  
Author(s):  
Jiapeng Long ◽  
Sanxi Li ◽  
Bing Liang

Purpose This paper aims to study a new halogen-free flame retardant that was prepared and characterised. Design/methodology/approach The phenyl phosphinic arid di-4-[1-(4-pheny phodphonic acid monophenyl ester-yl)-methyl-ethyl] phenyester dimelaminium (PDEPDM) was synthesised using phenylphosphonic dichloride, melamine, bisphenol A, triethylamine and dichloromethane via solvent-based reaction, that was added into the polyethylene to test flame performance. The chemical structures of PDEPDM were characterised by 1H nuclear magnetic resonance spectroscopy, mass spectrometry and Fourier transform infrared spectrometer. The thermal stability, mechanical and flame properties, and morphology for the char layer of composite materials were separately investigated using thermogravimetric analysis, tensile and charpy impact tests, limiting oxygen index (LOI) and UL-94 HB flammability standard and scanning electron microscope. Findings The results showed that the PDEPDM had been prepared successfully. When the intumescent fame retardant was added into the PE, the LOI of composite material was improved. Research limitations/implications The PDEPDM can be prepared successfully and can improve the flame resistance of composite material. Practical implications The PDEPDM has excellent flame-retardant properties and produce no toxic fumes when burnt in case of fire. Originality/value Under the optimal conditions, when the 32 per cent (Wt.%) PDEPDM was added into the PE, the LOI was 29.8, tensile strength and impact strength were 10.06 MPa and 16.77 kJ/m2.

e-Polymers ◽  
2019 ◽  
Vol 19 (1) ◽  
pp. 235-243 ◽  
Author(s):  
Lin Liu ◽  
Rui Lv

AbstractA DOPO (9,10-dihydro-9-oxa-10-phosphaphen-anthrene-10-oxide)-based halogen-free flame retardant (ODOPM-CYC) was synthesized and incorporated in rigid polyurethane foam (RPUF). The structure of ODOPM-CYC was characterized by Fourier transform infrared spectra (FTIR), 1H NMR and 31P NMR. The effects of ODOPM-CYC on the flame resistance, mechanical performances, thermal properties and cell structure of RPUF were also investigated. The results showed that the incorporation of ODOPM-CYC strikingly enhanced flame retardant properties of RPUF. The flame retarded RPUF acquired a limiting oxygen index (LOI) value of 26% and achieved UL-94 V-0 rating with the phosphorus content of 3 wt%. The smoke production rate (SPR) also showed an obvious decrease and total smoke release (TSR) was 39.8% lower than that of neat RPUF. Besides, the results demonstrated that the incorporation of ODOPM-CYC provided RPUF better thermal stability but did not show any obvious influence on its thermal conductivity.


2017 ◽  
Vol 46 (3) ◽  
pp. 172-180 ◽  
Author(s):  
Bing Liang ◽  
Jiao Lv ◽  
Gang Wang ◽  
Tsubaki Noritatsu

Purpose The purpose of this paper is to prepare a novel halogen-free intumescent flame retardant (IFR) BHPPODC (benzene hydroquinone phosphorous oxy dichloride cyanuric chloride) for application to epoxy resin (EP) and study their mechanical and flame-retardant performance. Design/methodology/approach The IFR was synthesised by phenylphosphonic dichloride, hydroquinone and cyanuric chloride via solvent reaction, and the structure was fully characterised by proton nuclear magnetic resonance (1H-NMR), mass spectrometry (MS) and Fourier transform infrared (FT-IR) spectroscopy. The thermal stability, mechanical and flame properties and morphology of the char layer of the flame-retardant EP was investigated by using thermogravimetric analysis (TGA), tensile and Charpy impact tests, limiting oxygen index (LOI) and vertical burning test (UL-94) and scanning electron microscopy (SEM). Findings Results of the LOI indicated that the halogen-free flame retardant as an additive exhibits very good flame-retardant effects. The results showed that the addition of IFR improved the flame resistance properties of epoxies resin composites, and the residual char ratio at 800°C significantly increased. Research limitations/implications The IFR can be prepared successfully and can improve the flame-retardant performance. Practical implications This contribution can provide a high flame retardant performance and has minimal impact on the mechanical performance of the BHPPODC/EP composition. Originality/value This study showed that flame-retardant BHPPODC has an effective flame effect under optimal conditions. When the 12 Wt.% IFR was added to the EP, the LOI was 29.1 and the UL-94 rank can reach V-0 rank, the tensile strength was 83.86 MPa and the impact strength was 8.82 kJ/m2.


2015 ◽  
Vol 1115 ◽  
pp. 406-409 ◽  
Author(s):  
Fatimah A’thiyah Sabaruddin ◽  
Noorasikin Samat ◽  
A.I.H Dayang Habibah

It is known that polymeric materials are easily to get on fire due to their chemical structures. Thus the flame retardant material such as aluminium hydroxide (ATH) is used to improve the flame retardancy property of polymers. Polypropylene (PP) with various amount of nanosized ATH particles of (5, 10, 20, 30, 40 wt%) were compounded with an extruder machine. The effects of two different type of coupling agent (3-Aminopropyltriethoxysilane (APS) and Maleic anhydride grafted polypropylene (MAPP)) on the flame retardant properties were compared. All samples were characterized with two flame tests; the limiting oxygen index (LOI) and UL94 horizontal burning test (UL94 HB). It is found that both tests showed improvement on the flame resistance properties of the nanocomposites, mainly at high ATH loadings. Type of coupling agents affects the flame retardancy properties of PP/ATH nanocomposites.


2015 ◽  
Vol 1107 ◽  
pp. 131-136
Author(s):  
A.I.H.Dayang Habibah ◽  
Abd Rahim Ruhida

Legislation on fire safety requirements especially in the USA and UK has been the driving force behind the use of halogen-free flame retardants (FR) in recent years. The present study describes the effect of inorganic fillers, namely aluminium hydroxides (ATH) on epoxidized natural rubber (ENR) in order to increase its flame retardant capability. Two different types of ATH, a standard type Apyral 60 CD (ATH 60) and a submicron sized Apyral 200 SM (ATH 200) were used. The flame-retardant ENR composite was characterized by limiting oxygen index (LOI), UL-94V, and thermogravimetric analysis (TGA) to study the combustion behavior and thermal stability. The finer particles size (ATH 200) as expected produced better flame retardant properties (measured by LOI) compared to ATH 60; however, the difference between the values is marginal. It was also observed that a combination of 100 pphr ATH 200 and 60 pphr ATH 60 gave the highest LOI value (29.4%) in ENR compounds. The compound was V0 rated in UL-94V burn test. Even at the higher loading, it was also found that the compound exhibited lower viscosity indicating its easier processability.


Polymers ◽  
2018 ◽  
Vol 11 (1) ◽  
pp. 48 ◽  
Author(s):  
Muhammad Maqsood ◽  
Gunnar Seide

Starch, being a polyhydric compound with its natural charring ability, is an ideal candidate to serve as a carbonization agent in an intumescent system. This charring ability of starch, if accompanied by an acidic source, can generate an effective intumescent flame retardant (IFR) system, but the performance of starch-based composites in an IFR system has not been tested in detail. Here, we describe a PLA-based IFR system consisting of ammonium polyphosphate (APP) as acidic source and cornstarch as carbon source. We prepared different formulations by melt compounding followed by molding into sheets by hot pressing. The thermal behavior and surface morphology of the composites was investigated by thermogravimetric analysis and scanning electron microscopy respectively. We also conducted limiting oxygen index (LOI), UL-94, and cone calorimetry tests to characterize the flame-retardant properties. Cone calorimetry revealed a 66% reduction in the peak heat release rate of the IFR composites compared to pure PLA and indicated the development of an intumescent structure by leaving a residual mass of 43% relative to the initial mass of the sample. A mechanism of char formation has also been discussed in detail.


2020 ◽  
Vol 993 ◽  
pp. 669-677
Author(s):  
Hui Min Ke ◽  
Ri Peng Zhu ◽  
Jing Hong Ma ◽  
Jing Hua Gong

Polyurethane (PU) superfine fiber leathers have been widely used in people's life. However, the flammability brings potential risks to their application. Therefore, more and more attention has been paid to the flame retardant modification of PU leathers. In the 1980s, researchers found that some brominated flame retardants produced dioxins during combustion. In 2007, the EU began implementing the REACH regulation, which restricted the use of certain halogenated flame retardants, so a majority of studies focused on halogen-free flame retardant modification. In addition, the halogen-free flame retardant PU should own a better alkali resistance, because alkali treatment is needed in the forming process of the superfine fiber leather. In this paper, two different halogen-free flame retardants were blended with solvent-based PU. The flame retardant properties and alkali resistance of the flame retardant PU were studied by limiting oxygen index (LOI) test, vertical burning (UL-94) test, and thermogravimetry-infrared spectroscopy (TG-FTIR). It was found that BY-90 system flame retardant could be uniformly dispersed in the PU matrix. And when its additive volume was 27%, the LOI value of the flame retardant PU was 27.1%, the vertical burning test could reach V-0 level. Moreover, it also had good alkali resistance. The LOI value remained at 26.1% after the alkali treatment at 90 °C for 40 min in the 30g/L NaOH solution.


2013 ◽  
Vol 2013 ◽  
pp. 1-8 ◽  
Author(s):  
Jie Liu ◽  
Jiayou Xu ◽  
Kaidan Li ◽  
Yongheng Chen

A novel charring agent, poly(p-ethylene terephthalamide) (PETA), for halogen-free flame retardant polypropylene was synthesized by using p-phthaloyl chloride (TPC) and ethylenediamine through solution polycondensation at low temperature, and the effects of PETA on flame retardance of polypropylene (PP)/IFR systems were studied. The experimental results showed that PETA could considerably enhance the fire retardant performance as proved by evidence of the increase of limiting oxygen index (LOI) values, the results of UL-94 tests, and cone calorimeter tests (CCT). Fourier transform infrared spectroscopy (FTIR) and scanning electron microscope (SEM) demonstrated that an appropriate amount of PETA could react with PP/IFR system to form cross-link network; a more compact char layer could be formed which was responsible for the improved thermal and flame retardant properties of PP/IFR systems. However, the superfluous amount of PETA would play the negative role.


Materials ◽  
2020 ◽  
Vol 13 (17) ◽  
pp. 3656
Author(s):  
Hangfeng Yang ◽  
Hangbo Yue ◽  
Xi Zhao ◽  
Minzimo Song ◽  
Jianwei Guo ◽  
...  

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.


Molecules ◽  
2019 ◽  
Vol 24 (8) ◽  
pp. 1513 ◽  
Author(s):  
Maqsood ◽  
Langensiepen ◽  
Seide

The objective of this study is to assess the efficiency of biobased carbonization agent in intumescent formulations (IFRs) to examine the flame retardant properties of polylactic acid (PLA) composites and to investigate their melt-spinnability. We used phosphorous-based halogen free flame retardant (FR) and kraft lignin (KL) as bio-based carbonization agent. After melt compounding and molding into sheets by hot pressing various fire related characteristics of IFR composites were inspected and were characterized by different characterization methods. It was fascinating to discover that the introduction of 5−20 wt% FR increased the limiting oxygen index (LOI) of PLA composites from 20.1% to 23.2−33.5%. The addition of KL with content of 3−5 wt% further increased the LOI up to 36.6−37.8% and also endowed PLA/FR/KL composites with improved anti-dripping properties. Cone calorimetry revealed a 50% reduction in the peak heat release rate of the IFR composites in comparison to 100% PLA and confirmed the development of an intumescent char structure containing residue up to 40%. For comparative study, IFR composites containing pentaerythritol (PER) as a carbonization agent were also prepared and their FR properties were compared. IFR composites were melt spun and mechanical properties of multifilament yarns were tested. The analysis of char residues by energy dispersive X-ray spectrometry (EDS) and SEM images confirmed that PLA/FR/KL composites developed a thicker and more homogeneous char layer with better flame retardant properties confirming that the fire properties of PLA can be enhanced by using KL as a carbonization agent.


2013 ◽  
Vol 750-752 ◽  
pp. 1087-1090 ◽  
Author(s):  
Yi Lun Tan ◽  
Liu Sun ◽  
Si Chun Shao ◽  
Jin Peng Fu ◽  
Zhi Han Peng

In this paper, a series of novel halogen compounds, melamine halogen acid salts were directly synthesized by melamine and halogen acid in water phase. The chemical structures of melamine halogen acid salts were characterized by Fourier-transform infrared spectroscopy (FT-IR), elemental analysis and1H-NMR. Meanwhile, the thermal properties of compounds were investigated by thermogravimetric analysis (TGA). The TGA results showed that melamine halogen acid salts had good thermostability during polymer processing. Futhermore, limiting oxygen index (LOI) and vertical burning test were used to study the flame retardant properties of composites blended by melamine halogen acid salts and polymer. The results revealed good flame retardancy that flame retardant polyethylene with 2 wt% melamine hydrobromide in total 8 wt% flame retardants got LOI value of 29.7% and reached UL 94 V-0 rating.


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