Synthesis of a phosphoramidate flame retardant and its flame retardancy on cotton fabrics

AbstractA phosphoramidate flame retardant (dimethyl N,N-bis(2-hydroxyletheyl)phosphoramidate, DMBHP) was synthesized and applied to cotton fabrics for enhancing the flame retardancy. The structure of DMBHP was characterized by FT-IR and NMR. The flame retardancy and combustion behavior of the treated cotton fabrics were evaluated using the vertical flammability test (VFT), limiting oxygen index (LOI), and the cone calorimetric test. Moreover, to further analyze the flame retardant action of DMBHP in cotton fabrics, thermal degradability of the treated fabrics, as well as the chemical structure, surface morphology, and element contents of the char residue of the DMBHP-treated fabrics were also evaluated. The results show that, after treating with DMBHP, the cotton fabrics acquired a LOI value from 18.1 to 31.1 with the concentration increasing to 30% and self-extinguished in VFT tests when treated with up to 15% DMBHP. Besides, the total heat release and the peak heat release rate of DMBHP (30%)-treated fabric decreased obviously compared with the pure cotton along with more residue retained. TG, SEM, and EDS results of treated cotton fabric and the corresponding residue after burning showed that DMBHP has the capability of enhancing char formation. In addition, DMBHP will confer cotton fabrics a certain durability against washing with the help of 1,2,3,4-butanetetracarboxylic acid (BTCA) and citric acid (CA).

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Flammability and thermal properties of cotton fabrics modified with a novel flame retardant containing triazine and phosphorus components

Textile Research Journal ◽

10.1177/0040517516652349 ◽

2016 ◽

Vol 87 (11) ◽

pp. 1367-1376 ◽

Cited By ~ 20

Author(s):

Chaohong Dong ◽

Zhou Lu ◽

Peng Wang ◽

Ping Zhu ◽

Xuechao Li ◽

...

Keyword(s):

Heat Release ◽

Flame Retardant ◽

Cotton Fabric ◽

Flame Retardancy ◽

Decomposition Temperature ◽

Cotton Fabrics ◽

Cone Calorimetry ◽

Limiting Oxygen Index ◽

Untreated Cotton ◽

Index Value

A novel formaldehyde-free flame retardant containing phosphorus and dichlorotriazine components (CTAP) for cotton fabrics was synthesized. As an active group, the dichlorotriazine could react with cotton fabric via covalent reaction. The addition of 20.7 wt% CTAP into the cotton fabric obtained a high limiting oxygen index value of 31.5%, which was 13.5% higher than the pure cotton fabric. The results of heat release rate, total heat release and effective heat combustion indicated that CTAP effectively imparted flame retardancy to cotton fabric by the cone calorimetry test. With respect to the untreated cotton fabrics, the treated cotton fabrics degraded at lower decomposition temperature and form a consistent and compact char layer, which could be observed by thermogravimetric analysis, Fourier transform infrared spectroscopy and scanning electron microscopy. Compared to the untreated cotton fabrics, CTAP performed an effective role in flame retardancy for treated cotton fabrics. Meanwhile, it stimulated the formation of char and promoted the thermal stability of treated cotton fabrics during combustion.

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Epoxy resin/cyanate ester composites containing DOPO and wollastonite with simultaneously improved flame retardancy and thermal resistance

High Performance Polymers ◽

10.1177/0954008319897095 ◽

2020 ◽

Vol 32 (6) ◽

pp. 710-718

Author(s):

Zhengzhou Wang ◽

Xin Gao ◽

Wenfeng Li

Keyword(s):

Heat Release ◽

Flame Retardant ◽

Flame Retardancy ◽

Oxygen Index ◽

Thermal Studies ◽

Cyanate Ester ◽

Total Heat Release ◽

Limiting Oxygen Index ◽

Peak Heat Release Rate ◽

Ul 94

Flame-retardant epoxy (EP) resin/cyanate ester (CE) composites were prepared with 9,10-dihydro-9-oxa-10-phosphaphenanthrene 10-oxide (DOPO) and wollastonite (Wo). The combustion behavior of the flame-retardant EP/CE composites was investigated by limiting oxygen index (LOI), UL-94, and cone calorimeter tests. It is found that the EP/CE composite containing 7 wt% DOPO and 3 wt% Wo (sample 7DO/3Wo/EP/CE) exerts the best flame retardancy (LOI 35.5% and UL-94 V-0 rating). The peak heat release rate and total heat release of sample 7DO/3Wo/EP/CE increase slightly, while total smoke release decreases about 14% compared with the EP/CE composite containing 10 wt% DOPO (sample 10DO/EP/CE). Thermal studies indicate that the glass transition temperature and temperature at 5% mass loss of sample 7DO/3Wo/EP/CE are higher than that of sample 10DO/EP/CE. Moreover, the mechanical properties of EP/CE composites were investigated.

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Flame resistant cellulosic substrate using banana pseudostem sap

Polish Journal of Chemical Technology ◽

10.1515/pjct-2015-0018 ◽

2015 ◽

Vol 17 (1) ◽

pp. 123-133 ◽

Cited By ~ 30

Author(s):

S. Basak ◽

Kartick. K. Samanta ◽

S. Saxena ◽

S.K. Chattopadhyay ◽

R. Narkar ◽

...

Keyword(s):

Flame Retardant ◽

Flame Retardancy ◽

Oxygen Index ◽

Propagation Rate ◽

Cotton Fabrics ◽

Limiting Oxygen Index ◽

Flame Retardant Property ◽

Flammability Test ◽

Flame Retardant Properties ◽

Mechanical Strengths

Abstract Flame retardancy was imparted in cellulosic cotton textile using banana pseudostem sap (BPS), an eco-friendly natural product. The extracted sap was made alkaline and applied in pre-mordanted bleached and mercerized cotton fabrics. Flame retardant properties of both the control and the treated fabrics were analysed in terms of limiting oxygen index (LOI), horizontal and vertical flammability. Fabrics treated with the non-diluted BPS were found to have good flame retardant property with LOI of 30 compared to the control fabric with LOI of 18, i.e., an increase of 1.6 times. In the vertical flammability test, the BPS treated fabric showed flame for a few seconds and then, got extinguished. In the horizontal flammability test, the treated fabric showed no flame, but was burning only with an afterglow with a propagation rate of 7.5 mm/min, which was almost 10 times lower than that noted with the control fabric. The thermal degradation and the pyrolysis of the fabric samples were studied using a thermogravimetric analysis (TGA), and the chemical composition by FTIR, SEM and EDX, besides the pure BPS being characterized by EDX and mass spectroscopy. The fabric after the treatment was found to produce stable natural khaki colour, and there was no significant degradation in mechanical strengths. Based on the results, the mechanism of imparting flame retardancy to cellulosic textile and the formation of natural colour on it using the proposed BPS treatment have been postulated.

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Synthesis and characterization of flame-retardant-wrapped carbon nanotubes and its flame retardancy in epoxy nanocomposites

Polymers and Polymer Composites ◽

10.1177/09673911211024582 ◽

2021 ◽

pp. 096739112110245

Author(s):

Jiangbo Wang

Keyword(s):

Carbon Nanotubes ◽

Heat Release ◽

Flame Retardant ◽

Flame Retardancy ◽

Total Heat Release ◽

Pristine Cnts ◽

Peak Heat Release Rate ◽

Ep Matrix ◽

Better Than

A novel phosphorus-silicon containing flame-retardant DOPO-V-PA was used to wrap carbon nanotubes (CNTs). The results of FTIR, XPS, TEM and TGA measurements exhibited that DOPO-V-PA has been successfully grafted onto the surfaces of CNTs, and the CNTs-DOPO-V-PA was obtained. The CNTs-DOPO-V-PA was subsequently incorporated into epoxy resin (EP) for improving the flame retardancy and dispersion. Compared with pure EP, the addition of 2 wt% CNTs-DOPO-V-PA into the EP matrix could achieve better flame retardancy of EP nanocomposites, such as a 30.5% reduction in peak heat release rate (PHRR) and 8.1% reduction in total heat release (THR). Furthermore, DMTA results clearly indicated that the dispersion for CNTs-DOPO-V-PA in EP matrix was better than pristine CNTs.

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Flame-retardant cotton fabrics modified with phosphoramidate derivative via electron beam irradiation process

Journal of Industrial Textiles ◽

10.1177/1528083719881816 ◽

2019 ◽

pp. 152808371988181

Author(s):

Ying Liu ◽

Li Zhou ◽

Fang Ding ◽

Shanshan Li ◽

Rong Li ◽

...

Keyword(s):

Electron Beam ◽

Flame Retardant ◽

Photoelectron Spectroscopy ◽

Electron Beam Irradiation ◽

Cotton Fabrics ◽

Beam Irradiation ◽

Limiting Oxygen Index ◽

Flammability Test ◽

Lower Temperature ◽

Irradiation Process

In this study, a novel flame-retardant diethyl methacryloylphosphoramidate containing phosphorus and nitrogen was synthesized and characterized by Fourier transform infrared and nuclear magnetic resonance. The synthesized compound was grafted onto cotton fabrics using electron beam irradiation and pad dry cure processes. Scanning electron microscope and X-ray photoelectron spectroscopy were used to characterize the surfaces of the modified cotton fabrics to confirm that diethyl methacryloylphosphoramidate was grafted on cotton fabrics successfully. Both electron beam–cotton and pad dry cure–cotton exhibited efficient flame retardancy which was proved by limiting oxygen index and vertical flammability test. Thermogravimetric analysis results showed that both electron beam-cotton and pad dry cure–cotton degraded at lower temperature and produced higher yields at 600℃. The tensile loss of electron beam–cotton was lower than that of pad dry cure–cotton, and within the acceptable range in flame retardant finishing.

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Synergistic Flame Retardant Effect of Barium Phytate and Intumescent Flame Retardant for Epoxy Resin

Polymers ◽

10.3390/polym13172900 ◽

2021 ◽

Vol 13 (17) ◽

pp. 2900

Author(s):

Linyuan Wang ◽

Yue Wei ◽

Hongbo Deng ◽

Ruiqi Lyu ◽

Jiajie Zhu ◽

...

Keyword(s):

Flame Retardant ◽

Epoxy Resin ◽

Flame Retardancy ◽

Barium Carbonate ◽

Environmentally Friendly ◽

Intumescent Flame Retardant ◽

Limiting Oxygen Index ◽

Application Range ◽

Peak Heat Release Rate ◽

Synergistic Flame Retardant

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.

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Novel P/Si Based Nanoparticles for Durable Flame Retardant Application on Cotton

10.21203/rs.3.rs-585202/v1 ◽

2021 ◽

Author(s):

Na Li ◽

Panpan Chen ◽

Dongni Liu ◽

Gaowei Kang ◽

Liu Liu ◽

...

Keyword(s):

Heat Release ◽

Flame Retardant ◽

Oxygen Index ◽

Dip Coating ◽

Gas Chromatography Mass Spectrometry ◽

Cotton Fibers ◽

Pyrolysis Gas ◽

Limiting Oxygen Index ◽

Potential Safety ◽

Ft Ir

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.

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Preparation of Mn2+ Doped Piperazine Phosphate as a Char-Forming Agent for Improving the Fire Safety of Polypropylene/Ammonium Polyphosphate Composites

Materials ◽

10.3390/ma14247589 ◽

2021 ◽

Vol 14 (24) ◽

pp. 7589

Author(s):

Fuqiang Dong ◽

Zhonglin Luo ◽

Biaobing Wang

Keyword(s):

Heat Release ◽

Flame Retardant ◽

Fire Safety ◽

Raw Materials ◽

Carbon Layer ◽

Ammonium Polyphosphate ◽

Manganese Acetate ◽

Limiting Oxygen Index ◽

Peak Heat Release Rate ◽

High Degree

A piperazine phosphate doped with Mn2+ (HP-Mn), as a new char-forming agent for intumescent flame retardant systems (IFR), was designed and synthesized using 1-hydroxy ethylidene-1,1-diphosphonic acid, piperazine, and manganese acetate tetrahydrate as raw materials. The effect of HP-Mn and ammonium polyphosphate (APP) on the fire safety and thermal stability of polypropylene (PP) was investigated. The results showed that the combined incorporation of 25 wt.% APP/HP-Mn at a ratio of 1:1 endowed the flame retardant PP (PP6) composite with the limiting oxygen index (LOI) of 30.7% and UL-94 V-0 rating. In comparison with the pure PP, the peak heat release rate (PHRR), the total heat release (THR), and the smoke production rate (PSPR) of the PP6 were reduced by 74%, 30%, and 70%, respectively. SEM and Raman analysis of the char residues demonstrated that the Mn2+ displayed a catalytic cross-linking charring ability to form a continuous and compact carbon layer with a high degree of graphitization, which can effectively improve the flame retardancy of PP/APP composites. A possible flame-retardant mechanism was proposed to reveal the synergistic effect between APP and HP-Mn.

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Influence of Magnesium Aluminate Nanoparticles on Epoxy-Based Intumescent Flame Retardation Coating System

Coatings ◽

10.3390/coatings10100968 ◽

2020 ◽

Vol 10 (10) ◽

pp. 968

Author(s):

Hatem Abuhimd ◽

Tentu Nageswara Rao ◽

Jung-il Song ◽

Prashanthi Yarasani ◽

Faheem Ahmed ◽

...

Keyword(s):

Heat Release ◽

Flame Retardant ◽

Magnesium Aluminate ◽

Coating System ◽

Limiting Oxygen Index ◽

Foaming Agents ◽

Peak Heat Release Rate ◽

Flame Retardation ◽

Coating Formulation ◽

Intumescent Flame Retardation

Ethylenediamine modified ammonium polyphosphate (EDA-MAPP) and charring-foaming agents (CFA) were prepared using a simple chemical method and further used to make intumescent flame retardant coatings based on epoxy resin. The content of MAPP and CFA was fixed at a ratio of 2:1. Nanoparticles of magnesium aluminate (MgAl2O4 NPs) have been introduced into the flame retardant coating formulation in various quantities to evaluate the promotional action of MgAl2O4 NPs with a flame retardant coating system. The promotional action of MgAl2O4 NPs on the flame retardant coating formulation was studied using a vertical burning test (UL-94V), limiting oxygen index (LOI), thermogravimetric analysis (TGA) and Fourier transform infra-red spectroscopy (FTIR). The UL-94V results indicated that the addition of MgAl2O4 effectively increased flame retardancy and met the V-0 rating at each concentration. The TGA results revealed that the incorporation of MgAl2O4 NPs at each concentration effectively increased the thermal stability of the flame retardant coating system. Cone-calorimeter experiments show that MgAl2O4 NPs effectively decreased peak heat release rate (PHRR) and total heat release (THR). The FTIR results indicated that MgAl2O4 NPs can react with MAPP and generate a dense char layer that prevents the transfer of oxygen and heat.

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Synthesis of a Novel Linear α, ω-Di (Chloro Phosphoramide) Polydimethylsiloxane and Its Applications in Improving Flame-Retardant and Water-Repellent Properties of Cotton Fabrics

Polymers ◽

10.3390/polym11111829 ◽

2019 ◽

Vol 11 (11) ◽

pp. 1829 ◽

Cited By ~ 2

Author(s):

Chaohong Dong ◽

Ling Sun ◽

Xingbo Ma ◽

Zhou Lu ◽

Pengshuang He ◽

...

Keyword(s):

Flame Retardant ◽

Flame Retardancy ◽

Free Water ◽

Water Repellency ◽

Cotton Fabrics ◽

Water Repellent ◽

Cone Calorimetry ◽

Limiting Oxygen Index ◽

Washing Durability ◽

Char Length

A novel linear α, ω-di (chloro phosphoramide)-terminated polydimethylsiloxane (CPN-PDMS) was successfully synthesized and utilized as a formaldehyde-free water-repellent and flame-retardant for cotton fabrics. The flame retardancy of treated cotton fabrics was estimated by limiting oxygen index (LOI) test, vertical flammability test, and cone calorimetry test. The cotton fabrics treated with 350 g/L CPN-PDMS obtained excellent flame retardancy with an LOI value of 30.6% and the char length was only 4.3 cm. Combustion residues were studied using Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and energy dispersive spectrometry (EDS) analysis. Results show that CPN-PDMS can effectively enhance water repellency and fire resistance of cotton fabrics. Furthermore, the breaking strength test and the whiteness test strongly prove that the tensile strength and whiteness of the treated cotton fabrics were slightly lower than that of the pure cotton fabrics. The wash stability test showed that after 30 laundering cycles, the treated cotton fabrics still had an LOI value of 28.5% and a water-repellent effect of grade 80, indicating that CPN-PDMS was an excellent washing durability additive. In summary, these property enhancements of treated cotton fabrics were attributed to the synergistic effect of silicon-phosphorus-nitrogen elements in CPN-PDMS.

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