scholarly journals Synthesis of a Compound Phosphorus-Nitrogen Intumescent Flame Retardant for Applications to Raw Lacquer

Polymers ◽  
2021 ◽  
Vol 13 (17) ◽  
pp. 2858
Author(s):  
Bing-Chiuan Shiu ◽  
Kunlin Wu ◽  
Ching-Wen Lou ◽  
Qi Lin ◽  
Jia-Horng Lin

Raw lacquer (RL) is a natural polymer compound with highly promising applications; however, its inflammable attribute restricts the industrial applications. In this study, melamine is used to formulate tri (1-melamine-2-propanol) phosphate (FR-1), after which it is synthesized with ammonium phosphate (FR-2) and diatomite to form a compound phosphorus-nitrogen intumescent flame retardant (IFR). Next, IFR is used as the filling agent that then cross-links with RL, and as such RL/IFR membranes are formed after the curing. The limiting oxygen index (LOI) measurement, the vertical combustion test (UL-94), the microshape calorimetric analysis (CCT), and the thermal gravimetric analysis (TGA) are conducted to examine the combustion resistance and thermal stability of the membranes. Fourier transform infrared spectroscopy (FT-IR) and electron scanning microscope (SEM) are performed to separately characterize the structure and compatibility; the mechanical properties of the membranes are also evaluated. The vertical combustion test results confirm that with 30 wt% of IFR, RL/IFR membranes acquire 12.3% higher LOI and a vertically combustion of V-0 level. The TGA indicates that RL/IFR membranes demonstrate a greater adhesion level, a higher rigidity, and better luster than pure RL membranes.

2012 ◽  
Vol 550-553 ◽  
pp. 2767-2772
Author(s):  
Xiu Yun Li ◽  
De Tian Liao ◽  
Han Bing Ma ◽  
Kang Lin Xu ◽  
An Bin Tang

An intumescent flame retardant (IFR) system containing phosphorus-silicon (EMPZR) and ammonium polyphosphate (APP) was used to improve the flame retardancy of poly(ethylene-co-vinyl acetate)(EVA). The influence of EMPZR contents on the flame retardance of EVA/EMPZR/APP composites has been studied. It was found that the reasonable mass ratio of EMPZR/APP in EVA/EMPZR/APP composites is 20/20, whose limiting oxygen index (LOI) value was improved from 19.0 for EVA to 28.6, and the burning grading reached to UL-94 V-0. The thermal behavior of EVA and IFR-EVA was investigated by dynamic thermo gravimetric analysis (TGA) at different heating rates and then the thermal degradation activation energies of EVA and IFR-EVA were determined by using Flynn-Wall-Ozawa method. Meanwhile, morphology of the char residue obtained from burning IFR-EVA in LOI test was studied through the scanning electron microscopy SEM observation, the rich compact char layer in which could explain the good flame retardance and the synergistic effect between EMPZR and APP.


Molecules ◽  
2020 ◽  
Vol 25 (24) ◽  
pp. 5978
Author(s):  
Riyazuddin ◽  
Samrin Bano ◽  
Fohad Mabood Husain ◽  
Jamal Akhter Siddique ◽  
Khadijah H. Alharbi ◽  
...  

Epoxy resins (EP) have been used as a thermos-setting material in the field of coating, casting, bonding agent, and laminating. However, a major drawback associated with its use is the lack of good flaming properties, and it is responsible for heavy smoke along with hazardous gases considerably limiting its uses in various fields. In this study, N-ethanolamine triazine-piperizine, a melamine polymer (ETPMP), was established as a new charring-foaming agent and was successfully synthesized with ethanolamine, piperizine, cyanuric chloride, and melamine as precursor molecules via the nucleophilic substitution reaction method. Elemental analysis and Fourier transform infrared (FTIR) spectroscopy analysis were applied to approve the synthesis of ETPMP and confirmation of its structure and characterization. The epoxy coating of intumescent flame retardant (IFR) was equipped by introducing ETPMP, ammonium polyphosphate (APP), and copper oxide (CuO) in multiple composition ratios. CuO was loaded at various amounts into the IFR-coating system as a synergistic agent. The synergistic action of CuO on IFR coatings was scientifically examined by using different analytical tests such as vertical burning test (UL-94V), limited oxygen index (LOI), thermal gravimetric analysis (TGA), cone calorimeter, and scanning electron microscope (SEM). The results showed that small changes in the amount of CuO expressively amplified the LOI results and enhanced the V-0 ratings in the UL-94V test. The TGA data clearly demonstrate that the inclusion of CuO can transform the thermal deprivation behavior of coatings with a growing char slag proportion with elevated temperatures. Information from cone calorimeter data affirmed that CuO can decrease the burning factors by total heat release (THR) together with peak heat release rate (PHRR). The SEM images indicated that CuO can enrich the power and compression of the intumescent char that restricts the movement of heat and oxygen. Our results demonstrate a positive influence of CuO on the epoxy-headed intumescent flame retardant coatings.


2014 ◽  
Vol 1033-1034 ◽  
pp. 931-936
Author(s):  
Cong Yan Chen ◽  
Rui Lan Fan ◽  
Guan Qun Yun

A novel intumescent flame retardant (IFR) containing ferrocene and caged bicyclic phosphate groups, 1-oxo-4-[4'-(ferrocene carboxylic acid phenyl ester)] amide-2, 6, 7-trioxa-1-phosphabicyclo- [2.2.2] octane (PFAM), was successfully synthesized. The synthesized PFAM were added to flammable polyurethane (PU) as flame retardants and smoke suppressants. The structure of PFAM was characterized by Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance (1H NMR) and elemental analysis. Thermal stability of PFAM was tested by themogravimetric analysis (TGA). The results revealed that PFAM had good thermal stability and high char weight, the char weight up to 54% at 600 °C. Flammability properties of PU/PFAM composites were investigated by limiting oxygen index (LOI) test and UL-94 test, respectively. The results of LOI tests showed that the addition of PFAM enhanced flame retardancy of PU. When the content of PFAM reaches to 3%, the LOI value is 22.2. The morphologies of the char for PU and PU/3% PFAM composite can be obtained after LOI testing were examined by SEM. The results demonstrated that PFAM could promote to form the compact and dense intumescent char layer. Experiments showed that, the PFAM application of polyurethane showed positive effect.


Polymers ◽  
2019 ◽  
Vol 11 (1) ◽  
pp. 71 ◽  
Author(s):  
Xueying Shan ◽  
Kuanyu Jiang ◽  
Jinchun Li ◽  
Yan Song ◽  
Ji Han ◽  
...  

A new P-N containing the flame retardant, which was namely N,N′-dibutyl-phosphate diamide (DBPDA), was synthesized and it was assembled into the cavity of β-cyclodextrin (β-CD) to form an inclusion complex (IC). The structure and properties of IC were characterized by Fourier transform infraredspectroscopy (FTIR), wide-angle X-ray diffraction (WAXD), 1H nuclear magnetic resonance (1H NMR), scanning electron microscopy with X-ray microanalysis (SEM-EDS), differential scanning calorimeter (DSC) and thermal gravimetric analysis (TGA). 1H NMR and SEM-EDS were also used to identify the molar ratio of β-CD/DBPDA in IC and the results from the analyses indicated that their molar ratio was 1:1. In order to test the flame retardant effect of IC, it was added to epoxy (EP). IC was proposed to be able to act as an intumescent flame retardant (IFR) system in EP through a combination of β-CD and DBPDA properties during the combustion process. β-CD is a biomass carbon source, which has the advantages of environmental protection and low cost. Furthermore, DBPDA is both a source of acid and gas. When IC was heated, IC had the advantage of acting as both a carbon source and foam forming agent, while the DBPDA component were able to directly generate phosphoric acid and NH3 in situ. The impact of IC in low additive amounts on flame retardancy of EP was studied by the cone calorimeter test. When only 3 wt % IC was incorporated, the peak values of heat release rate (pHRR) and smoke production rate (pSPR) of EP were reduced by 22.9% and 33.3% respectively, which suggested that IC could suppress the heat and smoke release efficiently.


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.


2011 ◽  
Vol 391-392 ◽  
pp. 204-208
Author(s):  
Xiao Ping Hu ◽  
Yu Yang Guo ◽  
Quan Min Xu ◽  
Hui Min Heng ◽  
Liang Jun Li

A novel intumescent flame retardant oligomer containing phosphorous-nitrogen structure (PSPTR) was synthesized and characterized by Fourier Transform Infrared (FTIR) and Mass Spectrometry (MS). The thermal behavior of PSPTR was investigated by thermogravimetric analysis (TGA). The TGA data shows that PSPTR has a high initial temperature of thermal degradation and a high char residue of 41.18wt% at 700 . A novel intumescent flame retardant (IFR) system, which is composed of PSPTR and novolac phenol (NP), was used to impart flame retardancy of ABS. The combustion behaviors of the ABS/IFR composites were investigated by Limiting Oxygen Index (LOI) and UL-94 tests. When the content of IFR (PSPTR:NP=1:1 mass ratio) is 30 wt%, the LOI value of ABS/IFR reaches 28.2, and the vertical burning test reaches UL-94 V-1 rating.


Polymers ◽  
2021 ◽  
Vol 13 (17) ◽  
pp. 2900
Author(s):  
Linyuan Wang ◽  
Yue Wei ◽  
Hongbo Deng ◽  
Ruiqi Lyu ◽  
Jiajie Zhu ◽  
...  

Recently, widespread concern has been aroused on environmentally friendly materials. In this article, barium phytate (Pa-Ba) was prepared by the reaction of phytic acid with barium carbonate in deionized water, which was used to blend with intumescent flame retardant (IFR) as a flame retardant and was added to epoxy resin (EP). Afterward, the chemical structure and thermal stability of Pa-Ba were characterized by Fourier transform infrared (FTIR) spectroscopy and thermogravimetric analysis (TGA), respectively. On this basis, the flammability and flame retardancy of EP composites were researched. It is shown that EP/14IFR/2Ba composite has the highest limiting oxygen index (LOI) value of 30.7%. Moreover, the peak heat release rate (PHRR) of EP/14IFR/2Ba decreases by 69.13% compared with pure EP. SEM and Raman spectra reveal the carbonization quality of EP/14IFR/2Ba is better than that of other composites. The results prove that Pa-Ba can cooperate with IFR to improve the flame retardancy of EP, reducing the addition amount of IFR in EP, thus expanding the application range of EP. In conclusion, adding Pa-Ba to IFR is a more environmentally friendly and efficient method compared with others.


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.


Polymers ◽  
2018 ◽  
Vol 10 (8) ◽  
pp. 871 ◽  
Author(s):  
Rong-Kun Jian ◽  
Long Xia ◽  
Yuan-Fang Ai ◽  
De-Yi Wang

The aim of this work is to prepare flame-retardant biobased poly(lactic acid) materials through incorporating a novel flame retardant dihydroxy-containing ammonium phosphate (DAP) derived from 2-chloro-5,5-dimethyl-1,3,2-dioxaphosphinane-2-oxide (DOP) and 2-amino-2-methyl-1,3-propanediol (AMPD). Interestingly, PLA modified with only 0.5% DAP passed UL-94 V-0 rating, and possessed a limiting oxygen index (LOI) value of 24.6%, which would further increase with the increasing loading of DAP. PLA/DAP did not exhibit obviously improved results in terms of heat release rate (HRR), as the loading of DAP was relatively low. It was found that DAP showed little effect on the thermal stability of PLA and the onset decomposition temperatures of PLA and PLA/DAP blends were very close. Besides, the degree of crystallization increased because of the plasticized effect of DAP. Based on the analyses of flame-retardant mechanism of DAP, it disclosed that DAP decomposed to generate incombustible compounds, such as water and ammonia, to dilute the concentration of oxygen and fuels, and then release some phosphorus-containing fragments that could produce phosphorus-containing free radicals to interrupt free-radical reactions, and finally noncombustible melt dripping was produced so as to bring away large amount of heat and stop the feedback of heat to the matrix.


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