scholarly journals Flame Retardant Waterborne Polyurethanes: Synthesis, Characterization, and Evaluation of Different Properties

2021 ◽  
Vol 12 (3) ◽  
pp. 3198-3214

A series of flame retardant waterborne polyurethanes (WBPUs) with varying NCO:OH mole ratio, i.e., isocyanate:hydroxyl groups, was synthesized using phosphorus-based polyester polyol and isophorone diisocyanate (IPDI). The phosphorus moiety was kept in the polymeric chain, which improves flame retardancy of the WBPU films. The prepolymer mixing process was adopted for the synthesis route of WBPU systems. The presence of structural-functional groups was confirmed by Fourier transform infrared spectroscopy and nuclear magnetic resonance spectroscopy. The thermal stability and percentage char yield were observed by TGA analysis. As a consequence of the existence of phosphorous moiety, these WBPUs also exhibit flame retardancy, which was examined by limiting oxygen index (LOI) and UL-94 test. All the samples show an increment in thermal stability with an increase in NCO:OH ratio. Maximum flame retardancy was obtained in FWP5 and FWP6 systems with LOI value of 32%.

1993 ◽  
Vol 11 (5) ◽  
pp. 442-456 ◽  
Author(s):  
Jun Zhang ◽  
Michael E. Hall ◽  
A. Richard Horrocks

This paper is the first in a series of four which investigates the burning behaviour and the influence of flame retardant species on the flam mability of fibre-forming polymer and copolymers of acrylonitrile. A pressed powdered polymer sheet technique is described that enables a range of polymer compositions in the presence and absence of flame retardants to be assessed for limiting oxygen index, burning rate and char residue deter minations. The method offers a rapid, reproducible and convenient means of screening possible flame retardant systems, and LOI values compare favourably with those of films and fabrics comprising the same polymeric type. Burning rates, however, are sensitive to changes in physical sample character such as form (film vs. powder sheet) and density. Thus the technique forms an excellent basis for the generation of burning data which will enable comprehensive studies of acrylic polymer flammability and flame retardancy to be undertaken.


Author(s):  
Alif Walong ◽  
Bencha Thongnuanchan ◽  
Tadamoto Sakai ◽  
Natinee Lopattananon

Rubber nanocomposite foams based on 60/40 ethylene vinyl acetate (EVA)/natural rubber (NR) were melt-mixed with flame retardant silicon dioxide (SiO2) (20 parts per hundred rubber, phr), and foamed by compression molding process. In this study, the effect of mixing phenomena of SiO2 through two different compounding techniques such as direct mixing (DM) and phase selective mixing (PSM) methods on structure, thermal stability, combustility and flame retardancy of EVA/NR blend nanocomposite foams were investigated. DM method is a melt mixing of EVA, NR, layered silicate and SiO2, followed by foaming. PSM is a new method based on pre-mixing EVA with SiO2, then melt mixing of EVA/SiO2 masterbatch with NR and layered silicate, and finally foaming. Based on TEM technique, it was found that the SiO2 was exclusively located in dispersed NR phase for the sample prepared by DM method, and the SiO2 was preferably dispersed in continuous EVA matrix when PSM method was employed. However, the different mixing methods did not significantly alter their cellular structures. The thermal stability and char residue content of foamed samples with SiO2 increased obviously when compared with those of corresponding foams without SiO2. The results based on limiting oxygen index (LOI) test and oxygen bomb calorimetry indicated that the foams combined with SiO2 had better combustion resistance and flame retardancy due to barrier effect of thermally stable silicon-based char layer. Further, the SiO2 filled foamed system obtained from the PSM method showed a higher degree of improvement in thermal stability, combustion resistance and flame retardancy than that of DM method because the homogeneous dispersion of SiO2 in EVA matrix rather than the selective dispersion in NR phase. This resulted in the continuity of flame retardant EVA/SiO2 phase in the 60/40 EVA/NR nanocomposite foams, which exerted more efficient fire barrier of the silicon-based char layer.


2017 ◽  
Vol 748 ◽  
pp. 51-54
Author(s):  
Pei Bang Dai ◽  
Lin Ying Yang ◽  
Ting Zheng ◽  
Chang Qin ◽  
Qi Chen Tang

A rigid polyurethane (PU) flame retardant composite foam was prepared by the compounding of polyols and diisocyanates with a modified intumescent flame retardant (MIFR). The MIFR was based on the three components of intumescent flame retardant normally used and was modified in a surfactant TX-10 solution. The flame retardancy of the PU flame retardant composite foams were evaluated by using the limiting oxygen index (LOI), the UL-94 (vertical flame) test and scanning electron microscopy (SEM). When MIFR was fixed at 20.0 wt% in PU/MIFR composite foams, the MIFR could enhance the flame retardancy and pass V-0 rating of UL-94 test. The microstructures observed by SEM demonstrate that a suitable amount of MIFR can promote formation of compact intumescent charred layers in PU foams.


2011 ◽  
Vol 399-401 ◽  
pp. 1376-1380
Author(s):  
Li Hua You ◽  
Yin Yin Hui ◽  
Xiang Ning Shi ◽  
Zhi Han Peng

In this study, a novel phosphorus-nitrogen containing intumescent flame retardant (P-N IFR) poly(melamine 2-carboxyethyl(phenyl) phosphate)(PMCEP) was prepared via the reaction of 2-carboxyethyl (phenyl) phosphinic acid (CEPPA) and melamine (MEL) in two-steps. Meanwhile, the molecular structure of the chemical compound was determined by FTIR,1H-NMR and elemental analysis; and the thermal properties was investigated by means of TGA. Combustion studies revealed high limiting oxygen index (LOI) indicative of better flame-retardancy properties for PBT resin.


2012 ◽  
Vol 24 (8) ◽  
pp. 738-746 ◽  
Author(s):  
Rui Zhang ◽  
Xifu Xiao ◽  
Qilong Tai ◽  
Hua Huang ◽  
Jian Yang ◽  
...  

Lignin–silica hybrids (LSHs) were prepared by sol–gel method and characterized by Fourier transform infrared (FT-IR) spectra, X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). LSH and ammonium polyphosphate (APP) were added into poly(lactic acid) (PLA) as a novel intumescent flame-retardant (IFR) system to improve the flame retardancy of PLA. The flame-retardant effect of APP and LSH in PLA was studied using limiting oxygen index (LOI), vertical burning (UL-94) tests and cone calorimeter. The thermal stability of PLA/APP/LSH composites was evaluated by thermogravimetric analysis (TGA). Additionally, the morphology and components of char residues of the IFR-PLA composites were investigated by SEM and XPS. With the addition of APP/LSH to PLA system, the morphology of the char residue has obviously changed. Compared with PLA/APP and PLA/APP/lignin, a continuous and dense intumescent charring layer with more phosphor in PLA composites is formed, which exhibits better flame retardancy. All the results show that the combination of APP and LSH can improve the flame-retardant property and increase the thermal stability of PLA composites greatly.


2018 ◽  
Vol 36 (6) ◽  
pp. 535-545 ◽  
Author(s):  
Daikun Jia ◽  
Yi Tong ◽  
Jin Hu

Flame-retardant rigid polyurethane foams incorporating N,N-(pyromellitoyl)-bis-l-phenylalanine diacid ester glycol have been prepared. After adding N,N-(pyromellitoyl)-bis-l-phenylalanine diacid ester glycol, the density and compressive strength of the polyurethane foams were seen to decrease. The flame retardancy of the polyurethane foams has been characterized by limiting oxygen index, upper limit–94, and cone calorimeter tests. The polyurethane foam with 2.27 wt% N,N-(pyromellitoyl)-bis-l-phenylalanine diacid ester glycol gave a highest limiting oxygen index of 33.4%, and the peak heat release rate of polyurethane foam reduced to 19.5 kW/m2 from 47.6 kW/m2 of PU-0 without N,N-(pyromellitoyl)-bis-l-phenylalanine diacid ester glycol. Upper limit–94 revealed N,N-(pyromellitoyl)-bis-l-phenylalanine diacid ester glycol did not change the burning rating, and all polyurethane foams had passed V-0 rating. The thermal stability of polyurethane foams has been investigated by thermogravimetric analyzer. N,N-(pyromellitoyl)-bis-l-phenylalanine diacid ester glycol significantly increased the initial decomposition temperature of polyurethane foams and their residues. In addition, the morphology of residual char from the flame-retarded polyurethane foams after cone calorimeter tests has also been characterized by digital photographs. The results indicated that N,N-(pyromellitoyl)-bis-l-phenylalanine diacid ester glycol significantly enhanced the strength and compatibility of the char layer formed by the polyurethane foams. These results indicate that N,N-(pyromellitoyl)-bis-l-phenylalanine diacid ester glycol can improve both the quality and quantity of the char, which has a significant effect on the flame-retardant properties of the foam.


2020 ◽  
Vol 842 ◽  
pp. 314-325
Author(s):  
Bin Lin

Epoxy resin (EP) mortar usually used to repair the cracking of concrete structure under damp environment, but EP is extremely flammable, thus it’s extremely imperative to design a novel multifunction EP grouting materials with flame retardancy and waterproofness for the practical application. Targeting ingenious decoration of EP grouting materials, multiple flame retardant elements (phosphorus, nitrogen and fluorine) are concurrently introduced into a fire retardant and the fire retardant defined as DDM-FNP. The obtained DDM-FNP/EP grouting composite possess high thermal stability, flame retardancy and hydrophobicity. The limiting oxygen index (LOI) value of DDM-FNP/EP composites has a significant improve, which is increased from 26.7 (EP-0) to 35.8 (EP-4). Composites with more than 10 wt% of DDM-FNP could pass UL-94 V-0 rating without dripping. Compared with EP-0, the PHRR and THR of EP-4 are decreased by 31.1% and 21.6%, respectively. In addition, due to the introduction of the F element, the water contact angle of EP composites is changed from 75.2° (hydrophilicity) to 98.6° (hydrophobicity) after the introduction of a certain amount of DDM-FNP flame retardant. Therefore, this work provide a new perspective to design a multifunction EP grouting composite and improve the value of practical application on seepage prevention of tunnel.


10.6036/10327 ◽  
2022 ◽  
Vol 97 (1) ◽  
pp. 98-103
Author(s):  
XIAN WANG ◽  
JINLONG ZHUO ◽  
TIANQING XING ◽  
Xingran Wang

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


2020 ◽  
Vol 15 ◽  
pp. 155892501989894
Author(s):  
Xiaolu Sun ◽  
Jiayin Song ◽  
Jin Zhang ◽  
Jingyan Liu ◽  
Huizhen Ke ◽  
...  

Polyacrylonitrile-based pre-oxidized fibers with improved thermal stability, flame retardant, and mechanical properties were made from the pristine polyacrylonitrile fibers through chemical pretreatment followed by pre-oxidation in air. The morphological structure of the polyacrylonitrile-based pre-oxidized fibers was investigated by Fourier transfer infrared spectra, X-ray diffraction, scanning electron microscopy, and X-ray energy dispersive spectrometer. The changes of characteristic functional groups and chemical compositions confirmed the successful modification of the polyacrylonitrile fibers during pre-treatment. The grooves and cracks on the surface of polyacrylonitrile-based pre-oxidized fibers were remarkably decreased in comparison with that of pristine polyacrylonitrile fibers. The evolution of crystalline structure of the polyacrylonitrile fibers proved the occurrence of cyclization reactions during pre-oxidation. Meanwhile, thermal stability, flame retardant, and mechanical properties of polyacrylonitrile-based pre-oxidized fibers were also investigated by thermogravimetric analyzer, oxygen index meter, micro combustion calorimeter, and single fiber tensile tester, respectively. The results demonstrated that the polyacrylonitrile-based pre-oxidized fibers initially pre-treated by hydroxylamine hydrochloride, followed by monoethanolamine, had a high limiting oxygen index of 40.1 and breaking strength of 2.03 cN/dtex. The peak of heat release rate and total heat release of polyacrylonitrile-based pre-oxidized fibers decreased significantly while its charred residues increased, contributing to the improved flame retardant property.


2018 ◽  
Vol 42 (16) ◽  
pp. 13873-13883 ◽  
Author(s):  
Tianlu Xu ◽  
Chunling Zhang ◽  
Peihong Li ◽  
Xueyan Dai ◽  
Lijie Qu ◽  
...  

Polysiloxane foam (PSF) is a foam material with outstanding performance. However, the limiting oxygen index (LOI) of pure PSF is only 22.0 vol%, which can be attributed to combustible materials.


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