Novel flame retardancy effect of phenethyl-bridged DOPO derivative on epoxy resin

2017 ◽  
Vol 30 (6) ◽  
pp. 667-676 ◽  
Author(s):  
Wei Yan ◽  
Jie Yu ◽  
Mingqiu Zhang ◽  
Lijuan Long ◽  
Tao Wang ◽  
...  

A series of flame-retardant epoxy resins (EPs) containing either phenethyl-bridged 9 or 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide derivative (bisDOPO) were prepared. The flame-retardant properties of bisDOPO on EP composites were characterized by the limiting oxygen index (LOI), the UL-94 vertical burning, and the cone calorimeter test (CCT).The LOI of the EP/bisDOPO composites increased from 21.8% to 38.0%, and the hybrids with the 10 wt% bisDOPO obtained a V-0 rating in the UL94 vertical burning test. The char residue following the CCT showed intumescent structures with continuous and compact surfaces that can effectively suppress the spread of the flame and extinguish the fire. This was confirmed through both visual observation and scanning electron microscopy (SEM) measurements. The flame-retardant mechanism was studied by Fourier transform infrared spectroscope (FTIR), thermogravimetric analysis/infrared spectrometry, SEM/energy-dispersive X-ray, and pyrolysis-gas chromatography/mass spectrometry. Overall, bisDOPO was an effective flame retardant with potential applications within EP.

Polymers ◽  
2019 ◽  
Vol 11 (10) ◽  
pp. 1575 ◽  
Author(s):  
Peng Xu ◽  
Peiyuan Shao ◽  
Qing Zhang ◽  
Wen Cheng ◽  
Zichao Li ◽  
...  

A novel flame-retardant composite material based on zinc alginate (ZnAlg) and nano-cuprous oxide (Cu2O) was prepared through a simple, eco-friendly freeze-drying process and a sol-gel method. The composites were characterized and their combustion and flammability behavior were tested. The composites had high thermal stability and achieved nearly non-flammability with a limiting oxygen index (LOI) of 58. The results show remarkable improvement of flame-retardant properties in the ZnAlg/Cu2O composites, compared to ZnAlg. Furthermore, the pyrolysis behavior was determined by pyrolysis–gas chromatography–mass spectrometry (Py-GC-MS) and the flame-retardant mechanism was proposed based on the combined experimental results. The prepared composites show promising application prospects in building materials and the textile industry.


2019 ◽  
Vol 28 (1) ◽  
pp. 14-25
Author(s):  
Long Li ◽  
Yi Qian ◽  
Haiming Zhang ◽  
Haoyue Han ◽  
Peng Qiao

Red mud (RM) is one kind of basic solid waste produced from aluminum industry. RM is usually stored by the method of land stockpiling, which has caused serious environmental and safety issues. Bittern, a by-product of salt manufacture, is abundant in China. But the utilization rate is low, less than 20%. The disposal of waste bittern has become a challenge that attracts much attention in water industry. In this article, Mg/Al/Fe layered double hydroxides (Mg/Al/Fe-LDHs) were synthesized using the above two wastes by a coprecipitation method and characterized by X-ray diffraction (XRD) and scanning electron microscopy. The XRD results showed that LDHs were successfully synthesized. Then, the flame-retardant properties and thermal properties of Mg/Al/Fe-LDHs in ethylene vinyl acetate (EVA)/LDHs composites had been tested by cone calorimeter test (CCT), limiting oxygen index (LOI), smoke density test (SDT), and thermogravimetry–Fourier transform infrared spectrometry (TG-FTIR). The CCT results showed that the heat release rate (HRR) of the EVA/LDHs composites significantly decreased in comparison with that of pure EVA, and EVA2 sample showed the lowest peak value of HRR value of 204.59 kW m−2. The LOI results showed that EVA3 had a highest LOI value of 28.3% in all the samples. The SDT test indicated that Mg/Al/Fe-LDHs were beneficial to the smoke suppression performance of EVA composites. TG-IR results showed that EVA/LDHs composites had better thermal stability than EVA.


2019 ◽  
Vol 2019 ◽  
pp. 1-13
Author(s):  
Long Li ◽  
Yi Qian ◽  
Peng Qiao ◽  
Haoyue Han ◽  
Haiming Zhang

Bittern, as a byproduct of salt manufacture, is abundant in China. The researches and developments for seawater bittern have mainly focused on the reuse of magnesium, calcium, lithium, and boron. However, the utilization rate is less than 20%. The large amount of unused bittern has become a challenge that attracts much attention in academic and industry areas. In this paper, three kinds of layered double hydroxides (LDHs) were synthesized from bittern using a coprecipitation method and characterized by X-ray diffraction (XRD). The XRD results showed that the three kinds of LDHs(MgAl-LDHs, MgFe-LDHs and MgAlFe-LDHs) were successfully synthesized. Then, the flame retardant properties and thermal properties of the three LDHs in ethylene vinyl acetate (EVA)/LDHs composites had been tested by cone calorimeter test (CCT), limiting oxygen index (LOI), smoke density test (SDT), and thermogravimetry-Fourier transform infrared spectrometry (TG-IR). The CCT results showed that the heat release rate (HRR) of all three kinds of EVA/LDHs composites significantly decreased compared with that of pure EVA, and the EVA/MgAl-LDHs composites had the lowest PHRR value of 222.65 kW/m2. The LOI results showed that EVA/MgAl-LDHs composites had the highest LOI value of 29.8%. The SDT results indicated that MgAl-LDHs were beneficial to smoke suppression. TG-IR results showed that EVA/MgAl-LDHs composites had a better thermal stability.


2021 ◽  
pp. 095400832199241
Author(s):  
Zijin Luo ◽  
Zhe Chen ◽  
Jun Wei ◽  
Dongchao Wang ◽  
Han Chen ◽  
...  

A novel intumescent flame retardant, PPMD, was designed from phosphaphenanthrene and nitrogen heterocycles through the two-step gut reactions of 1,4-phthalaldehyde and 3-methyl-1-phe-nylpyrazol-5-ylamine. After determination of its structure by nuclear magnetic resonance and Fourier-transform infrared analyses, PPMD was added to an epoxy resin (EP) to facilitate a curing process. Thus, EP/PPMD samples with excellent transparency and flame retardancy were acquired. For example, the EP sample satisfied the UL-94 V-0 standard and achieved a limiting oxygen index value of 30.5% because of the incorporation of 5 wt% PPMD. The cone calorimeter test of the EP/5% PPMD sample revealed that its total smoke production (TSP) and total heat release (THR) values of EP/5% PPMD was only 22.5% and 56.4% of the control group, respectively. Moreover, the average effective heat of combustion (av-EHC) value of EP/5% PPMD was reduced by 34.1%, indicating that PPMD possessed high flame-inhibition activity and smoke suppression efficiency. The flame-retardant mechanisms of PPMD were also investigated in gas phase by pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) and in condensed phase by XPS and IR.


2021 ◽  
Author(s):  
Na Li ◽  
Panpan Chen ◽  
Dongni Liu ◽  
Gaowei Kang ◽  
Liu Liu ◽  
...  

Abstract Cotton fibers as original materials of cotton fabrics have a widely application due to its perfect hygroscopicity, air permeability and largest annual output. However, cotton materials have potential safety hazard during its application because of flammability (limiting oxygen index is about 18%). In order to improve the flame retardancy of cotton fibers and reduce the damage of its mechanical properties, novel P/Si based flame retardant (PFR) nanoparticles were synthesized by one-step radical polymerization. Vinyl phosphoric acid and tetramethyl divinyl disiloxane were introduced into the nanoparticles. The structure, morphology and thermal stability of PFR was characterized by fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM), thermogravimetric analysis test (TGA). Durable flame retardant cotton fibers were prepared by dip-coating and plasma induced crosslinking methods. Micro-calorimeter (MCC) characterization showed that the peak of heat release rate (pHRR) and the total heat release were reduced by 47.3% and 29.8% for modified cotton fibers compared with pure cotton fibers. Limiting oxygen index (LOI) of modified cotton fibers was increased to 27%. The residue carbon of modified cotton fibers was 19.0% at 700 o C, while the value of pure cotton fibers was 3.0%. Besides, durability of the modified cotton fibers was approved by cyclic washing test. In addition, flame retardant mechanism was revealed by collecting and analyzing condensed and gaseous pyrolysis products. The data of FE-SEM for residue carbon, FT-IR spectra of products at different pyrolysis temperatures and pyrolysis gas chromatography mass spectrometry (Py-GC-MS) showed that PFR was a synergistic flame retardant contained barrier and quenching effecting applied on cotton materials.


Polymers ◽  
2020 ◽  
Vol 12 (9) ◽  
pp. 2107
Author(s):  
Dongwei Yao ◽  
Guangzhong Yin ◽  
Qingqing Bi ◽  
Xu Yin ◽  
Na Wang ◽  
...  

In this study, we selected basalt fiber (BF) as a functional filler to improve the mechanical properties of ethylene vinyl acetate (EVA)-based flame retardant materials. Firstly, BF was modified by grafting γ-aminopropyl triethoxysilane (KH550). Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), scanning electron microscope (SEM), and energy dispersive X-ray spectroscopy (EDS) were used to comprehensively prove the successful modification of the BF surface. Subsequently, the modified BF was introduced into the EVA/magnesium hydroxide (MH) composites by melt blending. The limiting oxygen index (LOI), UL-94, cone calorimeter test, tensile test, and non-notched impact test were utilized to characterize both the flame retardant properties and mechanical properties of the EVA/MH composites. It was found that the mechanical properties were significantly enhanced without reducing the flame retardant properties of the EVA/MH composites. Notably, the surface treatment with silane is a simple and low-cost method for BF surface modification and the pathway designed in this study can be both practical and effective for polymer performance enhancement.


Polymers ◽  
2020 ◽  
Vol 12 (11) ◽  
pp. 2442
Author(s):  
Ji Su Kim ◽  
Ji Eun Song ◽  
Daeyoung Lim ◽  
Heejoon Ahn ◽  
Wonyoung Jeong

To produce flame retardant poly(acrylonitrile-co-vinylidene chloride) (PANVDC) fibers with limiting oxygen index (LOI) values above 28%, flame retardants are added to fibers. Because antimony trioxide (ATO) used widely for PANVDC is suspected as a carcinogen, non-toxic zinc hydroxystannate (ZHS) could be the alternative for reduction of ATO usage. Moreover, a flame retardant efficiency of the combination of ATO with ZHS could be expected because it was reported that ATO resists flame in the gas phase, whereas ZHS reacts in the condensed phase. Therefore, this study discussed the flame retardant mechanisms of ATO and ZHS in PANVDC, and evaluated the efficiency of the combination. PANVDC fibers with ATO and ZHS in 15 phr were produced by wet spinning. When ZHS was added, a more cyclized structure was detected (e.g., 1-methylnaphthalene) through pyrolysis−gas chromatography-mass spectrometry (Py-GC/MS). As a result of SEM-EDX analysis, Sb and Cl hardly remained in char layers of PANVDC-ATO; meanwhile, Zn, Sn, and Cl remained in that of PANVDC-ZHS. This implied that SbCl3 from reaction of ATO and HCl reacts in the gas phase, whereas ZnCl2 and SnCl2 from ZHS and HCl promotes the cyclization reaction of PANVDC in the condensed phase. The LOI values of PANVDC, PANVDC-ATO, and PANVDC-ZHS were 26.4%, 29.0%, and 33.5%, respectively. This suggests that ZHS is a highly effective for PANVDC. Meanwhile, the LOI of PANVDC containing ATO-ZHS mixture is 31.0%. The combination of ATO and ZHS exhibited no efficiency. The addition of ATO and ZHS slightly reduced the tenacities of the fibers, respectively, 3.11 and 3.75 from 4.42 g/den.


e-Polymers ◽  
2021 ◽  
Vol 21 (1) ◽  
pp. 299-308
Author(s):  
Jiawei Jiang ◽  
Ruifeng Guo ◽  
Haifeng Shen ◽  
Shiya Ran

Abstract In this work, a phosphorous-containing flame retardant, phenylphosphonate-based compound (EHPP), is synthesized by alcoholysis and hydrazinolysis of phenylphosphonic dichloride, which is subsequently introduced to ethylene-vinyl-acetate (EVA) copolymer to improve its flame retardant performance. The resultant compound was characterized by Fourier transform infrared (FTIR), 1H NMR, 13C NMR, and 31P NMR. The influence of the EHPP on the combustion behaviors of EVA is studied by limiting oxygen index (LOI), UL-94, and cone calorimeter test. The results show that 1 wt% EHPP can reduce peak heat release rate (PHRR) by 40%. Moreover, 2 wt% EHPP can increase LOI from 20.5% to 25.5%. Thermogravimetric analysis/infrared spectrometry (TGA-FTIR) was used to detect the gaseous products of EVA/EHPP to study the gaseous-phase flame retardant mechanism. The EHPP released phosphorus-containing radicals to capture highly active free radicals to improve the flame retardancy of EVA.


2018 ◽  
Vol 1 (1) ◽  
Author(s):  
Mingyang Du ◽  
Chunze He ◽  
Canhui Zhou

The effect of Isocyanate trimer on the flame retardancy mechanism of polyisocyanurate (PIR) foam was studied through 3 aspects including the mechanism of thermal decomposition stage in condensed phase, the barrier mechanism of carbon layer formation on the surface in condensed phase and the mechanism in gaseous phase by using infrared spectroscopy, scanning electron microscopy, thermal analysis, cone calorimeter, high temperature pyrolysis gas chromatography mass spectrometry. The results show that the trimer can improve the thermal stability of the PIR foam and is not easily decomposed in the combustion. The trimer can increase the carbon content of the PIR foam to 29.9% than that of the polyurethane (PU) foam. The carbon layer formed is denser, and it can retards heat and oxygen and thus improve the flame retardant properties; trimer can reduce the release of flammable polyol gas, decompose into more carbon dioxide which is inert gas and it has certain flame retardant effect in the gaseous phase.


2015 ◽  
Vol 30 (6) ◽  
pp. 816-826 ◽  
Author(s):  
Yiren Huang ◽  
Jianwei Yang ◽  
Zhengzhou Wang

Flame-retardant properties of ammonium polyphosphate (APP) and its two microcapsules, APP with a shell of melamine–formaldehyde (MF) resin (MFAPP) and APP with a shell of epoxy resin (EPAPP), were studied in styrene–butadiene–styrene (SBS). The results indicate that APP after the microencapsulation leads to an increase in limiting oxygen index in SBS compared with APP. When dipentaerythritol is incorporated into the SBS composites containing the APP microcapsules, a further improvement in flame retardancy of the composites is observed. The microencapsulation does not result in much improvement of mechanical properties. Moreover, the effect of a compatibilizer (SBS grafted with maleic anhydride) on flame-retardant and mechanical properties of SBS/APP composites was investigated.


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