scholarly journals Investigation of the Flammability and Thermal Stability of Halogen-Free Intumescent System in Biopolymer Composites Containing Biobased Carbonization Agent and Mechanism of Their Char Formation

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.

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.


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.


2014 ◽  
Vol 884-885 ◽  
pp. 208-211
Author(s):  
Chun Xia Li ◽  
Quan Ji ◽  
Cui Cui Song ◽  
Feng Yu Quan ◽  
Yan Zhi Xia

Cellulose-insoluble silicate (talcum powder) hybrid fibers with 10%, 20%, 30% silica contents were prepared by wet spinning. The flammabilities and combustion processes were evaluated by the limiting oxygen index (LOI) and cone calorimetry. The LOI results suggested that the hybrid fibers were flame retandant with the LOI value of 22, 25 and 27, as compared to 20 of pure cellulose fibers. Cone calorimetry showed that the rate of heat release value and total heat release value of hybrid fibers decreased. Hybrid fibers with 20% SiO2 loading is the best flame retardant sample. SEM studies of residues after cone calorimetry indicated that the hybrid fibers produced tight and hard residue crusts.


2020 ◽  
Vol 72 (4) ◽  
pp. 13-21
Author(s):  
Diana Serbezeanu ◽  
Tachita Vlad-Bubulac ◽  
Elena Hamciuc ◽  
Corneliu Hamciuc ◽  
Gabriela Lisa ◽  
...  

The present study aimed to design macromolecular architectures having imide core in the main chain and bearing two 9,10-dihydro-oxa-10-phosphaphenanthrene-10-oxide heterocycles in the side chain of each structural units as a synergetic two components key factor to induce attractive flame retardant properties in the resulted materials. The synthesis pathway consisted in the classical polycondensation reaction strategy using a phosphorus-containing diamine synthesized in the laboratory and three commercial dianhydrides co-monomers. The chemical structure confirmation of the phosphorus-containing polyimides has been performed by means of FTIR and NMR spectroscopy. The thermal stability of the products was introspected through TGA analysis. The char yields measured at 900oC ranged between 35% and 54%. Using these parameters limiting oxygen index values were theoretically calculated. Also, the microscale combustion calorimetry measurements have been conducted, in order to investigate the combustion mechanism of the synthesized phosphorus-containing polyimides.


2021 ◽  
Vol 5 (2) ◽  
pp. 11-17
Author(s):  
Anrong Huang ◽  
Jing Sun ◽  
Shanshan Luo ◽  
Heng Luo

Nylon 1212/organic montmorillonite (OMMT) nanocomposites were prepared using the melt compounding method. The morphology and dynamical mechanical properties of the nanocomposites were investigated using transmission electron microscope (TEM) and dynamic mechanical analysis (DMA). The storage modulus of nylon 1212/OMMT nanocomposites was increased with increasing OMMT. The flame retardant properties were characterized by cone calorimetry, scanning electron microscope (SEM) and X-ray photoelectron spectroscopy (XPS). The flame retardant properties were characterized using cone calorimetry, whereby nylon 1212/OMMT nanocomposites were improved compared with pure nylon 1212 because of the carbonaceous-silicate granular materials which were formed during combustion, thus proposing the flame retardant mechanism.


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.


2019 ◽  
Vol 2019 ◽  
pp. 1-15 ◽  
Author(s):  
Ning Lu ◽  
Pengchao Zhang ◽  
Ya’nan Wu ◽  
Danqing Zhu ◽  
Zhu Pan

This paper is aimed at assessing the fire retardancy and thermal stability of intumescent flame retardant (IFR) containing ammonium polyphosphate (APP), pentaerythritol (PER), and melamine (MEL). Zinc borate (ZB) was added at the loading of 2%, 4%, 6%, 8%, 10%, and 12% by weight of IFR. The sizes of investigated ZB fall in 3 ranges: 1-2 μm, 2-5 μm, and 5-10 μm. The performance of APP/PER/MEL was investigated by using thermogravimetry analysis (TGA), cone calorimeter test, Fourier-transform infrared (FTIR) spectroscopy, scanning electron microscopy, and energy-dispersive spectrometry. The results obtained from the above experiments show that the incorporation of ZB can improve the fire protection performance. A 77% decrease in total smoke production and 84.6% decrease in total heat release were achieved for the addition of 2 wt% ZB (2-5 μm) in the IFR coating. TGA results indicate an increased amount of char residue. Compared to the control IFR coating, the char residue of IFR containing 2 wt% ZB (2-5 μm) has increased approximately 1.5-fold, 10-fold, and 25-fold, at 600°C, 700°C, and 800°C, respectively. The effective char formation results in excellent smoke suppression. Regarding smoke suppression performance, the order for smoke density is IFR/ZB (2-5 μm) < IFR/ZB (5-10 μm) < IFR/ZB (1-2 μm), regardless of investigated loading levels. The decline of smoke suppression performance for IFR/ZB (5-10 μm) and IFR/ZB (1-2 μm) is believed to be due to the poor char formation, as a result of a weak interaction of APP, PER, MEL, and ZB. This weak interaction is caused by the decrease in the specific surface area and agglomeration of ZB particles for IFR/ZB (5-10 μm) and IFR/ZB (1-2 μm), respectively.


2013 ◽  
Vol 634-638 ◽  
pp. 1927-1930 ◽  
Author(s):  
Jia Chen ◽  
Ji Yan Liu ◽  
Xue Qing Liu ◽  
Shan Sun

In this paper, magnesium methylcyclohexylphosphinate (Mg(MHP)) was used as flame retardant for epoxy resin(EP).The flame retardancy and thermal stability of Mg(MHP)/EP composites have been studied. As a result, the composite with 20-25% Mg(MHP) can achieve the satisfying flame retardancy with the limiting oxygen index (LOI) of 29.05 % and passing the UL-94 V-0 rating. TG results showed that adding Mg(MHP) into EP leads to a increase in the onset temperature of degradation and depresses the thermal decomposition below around 470 °C. Beyond 470 °C, the residue char of the composites lost more quickly compared to neat EP. A preliminary study seem to conclude that Mg(MHP) acts as the condensed source by promoting the char formation below around 470 oC and as the gas source by vaporizing at higher temperature.


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.


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