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JOURNAL OF APPLIED POLYMER SCIENCE · 2022 ·Vol. 139 ·期 44 ·e53070 · IF 3.057

Durable flame-retardant cotton fabric modified by water-soluble C–N–P intumescent flame retardant

Yuanyu Ge,Zhenming Qi,Desheng Sha,Xiaosai Hu,Shiwen Liu

Intumescent flame retardant (IFR) is the new generation of environmentally friendly flame retardant. The improved water solubility of IFR enhances its application in cellulose-based textiles. A water-soluble carbon–nitrogen–phosphorus (C–N–P) ternary IFR (PTETP) was synthesized using cyanuric chloride (TCT), ethylene glycol (EG), and O-phosphoethanolamine (O-PEA) as starting materials. The burning performance of untreated and PTETP treated cotton fabrics was evaluated using vertical flammability test (VFT), limiting oxygen index (LOI), and cone calorimetry. The results indicate that with the increase of PTETP content, the flame retardant performance of cotton fabrics is gradually enhanced. The cotton fabric treated with 10 wt% PTETP shows no afterflame combustion, has a char length of 98 mm, and a LOI of 30.8%. Compared with pristine cotton fabric, the peak heat release rate (PHRR) and total heat release (THR) of the treated cotton fabric were reduced by 52.6% and 28.2%, respectively. Thermogravimetric (TG) shows that PTETP effectively improves the thermal stability and reduces the thermal decomposition temperature of cotton fabric, and even can increases the residual carbon rate by 20%. In addition, the employment of PTETP shows no harm on the tensile strength of cotton fabrics. After washing 20 times, LOI of flame-retardant cotton fabric still remained almost 26%.

研究领域: 材料科学 · 纺织工程
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JOURNAL OF FIRE SCIENCES · 2017 · IF 1.051

Halogen-free flame-retardant rigid polyurethane foam with a nitrogen–phosphorus flame retardant

Qianqiong Zhao,Congyan Chen,Ruilan Fan,Yong Yuan,Yalin Xing,Xiao Ma

A halogen-free flame retardant containing nitrogen and phosphorus, 2-[anilino-(6-oxobenzo[c][2,1]benzoxaphosphinin-6-yl)methyl]phenol (PDOP), has been synthesized by reaction of benzo[c][2,1]benzoxaphosphinine-6-oxide (DOPO) with 2-(N-phenyliminomethyl)phenol. Halogen-free flame-retardant rigid polyurethane foams (RPUF-PDOP) were prepared using PDOP as a flame retardant. The flammability was investigated using limiting oxygen index, a vertical burning test (UL-94), and a cone calorimeter. When PDOP (10 wt%) as flame retardant was added to RPUF (RPUF-PDOP10%), the limiting oxygen index value was increased from 18% to 27%, and a UL-94 V-0 rating was achieved; meanwhile, the peak heat release rate, total heat release, and the average mass-loss rates of RPUF-PDOP10% were reduced from 246 to 207 kW m−2, from 26.9 to 21.0 MJ/m2, and from 0.043 to 0.033 g/s, respectively. Especially, the initial decomposition temperature of RPUF-PDOP10% was decreased from 228°C to 209°C. The final residual char from decomposition of RPUF-PDOP10% was significantly increased up to 35.6%. The addition of PDOP did not markedly decrease the mechanical properties of the resulting flame-retardant RPUFs.

研究领域: 材料科学 · 化学工程
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POLYMER DEGRADATION AND STABILITY · 2014 · IF 2.633

Two novel phosphorus–nitrogen-containing halogen-free flame retardants of high performance for epoxy resin

Liqiang Gu,Guoan Chen,Youwei Yao

Two novel halogen-free flame retardants , DP-DDE and DP-DDS, were synthesized via a one-pot procedure based on the Pudovik reactions between 9,10-dihydro-9-oxa-10-phosphaphenanthrene 10-oxide (DOPO) and imines directly resulting from the condensation reactions of 3-methoxy-4-hydroxybenzaldehyde with two typical curing agents , 4,4′-oxydianiline (DDE) and 4,4′-diaminodiphenylsulfone (DDS), respectively. The fire-resistant properties of DP-DDE or DP-DDS modified epoxy resins (2,2-bis(4-glycidyloxyphenyl)propane) with 4,4′-methylenedianiline as hardener were been investigated by UL-94 vertical test. Their high flame-retarding performance has been found: the epoxy thermosets with a relatively low addition amount of DP-DDE or DP-DDS (on the account of phosphorus content of 0.75 wt.% or 0.73 wt.%) can reach UL-94 V-0 flammability rating. These thermosets demonstrated excellent thermal stability, high glass transition temperature ( T g  > 135 °C) and high char yields (>22% at 800 °C). Moreover, the thermal degradation kinetics of the flame retardants and their corresponding epoxy thermosets were studied based on Kissinger, Ozawa and FWO methods by thermogravimetric analysis .

研究领域: 材料科学 · 化学工程
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POLYMER · 2023 · IF 4.6

A novel halogen-free flame-retardant fabrication for the study of smoke suppression and flame retardancy of polystyrene

Xianting Wang,Hongyi Tu,Haofeng Xiao,Junyi Lu,Jie Xu,Guangxin Gu

A novel P–N flame-retardant (PON) was synthesized by nucleophilic substitution reaction using diphenyl phosphoryl chloride and piperazine as raw materials. Its chemical structure was characterized by Fourier transform infrared spectroscopy (FTIR), liquid-state nuclear magnetic resonance (NMR), high resolution mass spectrometry (HEMS) and elemental analysis , and its thermal stability by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). Subsequently, five char-forming agents, namely pentaerythritol (PER), chitosan (CTS), lignin (LI), graphene (GN) and expandable graphite (EG), were selected to form five intumescent flame-retardants in a 1:1 mass ratio with PON. Polystyrene (PS) composites were prepared by melt blending method. The synergistic effect of PON and different char-forming agents on thermal stability, combustion behavior and flame retardancy of PS composites were systematically investigated. The results showed that the PS/10% PON/10% EG composite had the highest limiting oxygen index (LOI) value of 25.8%, and the cone calorimetric test showed that the peak heat release rate (pHRR), total heat release rate (THR), and total smoke release (TSP) of the composite were reduced by 74.6%, 24.4% and 43.6%, respectively, compared with neat PS, and this composite exhibited the most excellent flame retardancy. Finally, the flame-retardant mechanism of PS/10% PON/10% EG composite was discussed and proposed by the results of scanning electron microscope (SEM), thermogravimetric analysis coupled to Fourier transform infrared spectroscopy (TG-IR), and pyrolysis-gas chromatography-mass (PY-GC/MS) measurements in detail.

CAS / MDL: 7782-42-5
研究领域: 材料科学 · 化学工程
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POLYMER DEGRADATION AND STABILITY · 2024 · IF 6.3

The synthesis and properties of an intumescent zinc-chelated organometallic flame retardant

Tianyu Liu,Ying Tao,Xiuyuan Ni

Organometallic flame retardants (OFRs) are currently attracting intensive attention. Here, we synthesized a new zinc-chelated OFR, ZnDSi, which was incorporated with phosphorus, silicon, and nitrogen functional moieties. The resulting ZnDSi exhibited strong intumescent properties upon heating and demonstrated high thermal stability, with a decomposition temperature (T d, 5 % ) of 349 °C, making it suitable for the melt-processing of most engineering plastics. Comparative experiments demonstrated that the chelated zinc converted the properties of the resultant OFR, including its intumescence, thermostability and hydrophobicity. The ZnDSi was tested in polyamide 66 (PA66) for the flame-retardant properties. Incorporating 10 wt% of ZnDSi into PA66 attained a limiting oxygen index of 29.1 %, accompanied by the reduction of the peak heat release rate by 35.0 % and total heat release by 28.2 % when compared to the pure PA66 sample, according to the cone calorimeter tests. Mechanism investigation was conducted to probe into the interactions between zinc and organic components through a custom apparatus for pyrolytic gas analysis, and it was found that zinc could reduce the soot release by suppressing the formation of the soot precursors during the pyrolysis. This work contributes to a deeper understanding of how metal elements function in OFR systems, which may conduce to developing OFRs with advanced performance.

CAS / MDL: 35948-25-5
研究领域: 材料科学 · 化学工程
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COMPOSITES PART A-APPLIED SCIENCE AND MANUFACTURING · 2016 · IF 3.719

Synergistic flame retardancy effect of graphene nanosheets and traditional retardants on epoxy resin

Shan Liu,Zhengping Fang,Hongqiang Yan,Venkata S. Chevali,Hao Wang

Novel non-toxic halogen-free flame retardants are replacing traditional flame retardants in polymer and polymer matrix composite structures. In this study, graphene nanosheet (GNS) is investigated in combination with traditional layered double hydroxide (LDH), layered rare-earth hydroxide (LRH), and phosphorus-based flame retardant (DOPO) to enhance the flame retardancy of epoxy resin. A synergistic flame retardancy effect is achieved in GNS/LDH and GNS/DOPO systems where combined GNS and LDH increased the viscosity of the epoxy melt, and limited the flame propagation through inhibition of dripping. The limiting oxygen index of epoxy increased from 15.9 to 23.6 with addition of 0.5   wt.% each of GNS and LDH. With the addition of 2.5   wt.% of both GNS and LDH, the total heat release of epoxy resin also reduced from 33.4   MJ/m 2 to 24.6   MJ/m 2 . The synergistic effect of GNS and DOPO adopted a different mechanism. The addition of 2.5   wt.% of GNS and DOPO reduced the peak heat release rate from 1194   kW/m 2 to 396   kW/m 2 , and the total heat release rate from 72.5   MJ/m 2 to 48.1   MJ/m 2 . The synergistic mechanisms of the flame retardants were closely analyzed and correlated with the flame retardant properties.

CAS / MDL: 19598-90-4 35725-34-9
研究领域: 材料科学 · 高分子化学
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CHEMICAL ENGINEERING JOURNAL · 2021 · IF 13.273

Interfacial flame retardant unsaturated polyester composites with simultaneously improved fire safety and mechanical properties

Shenghe Zhang,Fukai Chu,Zhoumei Xu,Yifan Zhou,Weizhao Hu,Yuan Hu

The low flame retardant efficiency and poor interfacial property are the main problems that confine the wide application of glass-fiber reinforced unsaturated resin (GUPR) composites. Herein, these problems are effectively solved by grafting modified silane coupling agent on the surface of glass fiber and adding multi-element hybrid flame retardant to matrix. Firstly, phosphorus-containing flame retardant interface modifier (PKH550) and Sulfur-containing flame retardant (PCH 3 -S) were synthesized, and the structures were confirmed by Nuclear Magnetic Resonance spectroscopy (NMR) of 1 H and 31 P. Then PKH550 was successfully grafted on the surface of glass-fiber. Notably, compared with PGF/UPR 20% which had no rating in UL-94 test, the use of PKH550 modified glass-fiber made MGF/UPR 20% reached the V0 rating, and the limiting oxygen index (LOI) value was as high as 38%. In addition, with the increase addition of PCH 3 -S, the flame retardant properties of GUPR composites were gradually improved. Finally, the mechanical properties of GUPR composites had been improved further by the plasma method. Compared with the 296.93 MPa tensile strength of PGF/UPR, the tensile strength of P-PGF/UPR prepared after plasma treatment of glass-fiber increased to 319.27 MPa. This work provides a new angle to simultaneously improve the fire safety performance and mechanical properties of materials, which will not only be limited to the application of unsaturated resins, but can also have a rather good application prospects in other flame-retardant materials.

研究领域: 材料科学 · 高分子科学 · 复合材料 · 消防安全工程
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Polymers · 2023 ·Vol. 15 ·期 7 ·1655 · IF 5

Flame Retardancy of Epoxy Resins Modified with Few-Layer Black Phosphorus

Yongzheng Zhao,Yan Li,Jiaxuan Li,Yifan Xiao,Wenmin Mu,Zhongwei Wang,Liang Song,Jinhong Yu

Few-layer black phosphorus (BP)- and red phosphorus (RP)-modified diglycidyl ether of bisphenol A-based epoxy resins (EP) was prepared with 4,4′-diaminodiphenylsulfone as a curing agent. The thermal stability and flame-retardant properties of the modified EPs were compared. Both BP and RP were able to improve the flame-retardant properties of EPs, while the BP showed higher flame-retardant efficiency than RP. As a two-dimensional nanomaterial, BP exhibited good compatibility, high flame-retardant efficiency, and negligible impact on the mechanical and thermal stability of EP. Pyrolysis-gas Fourier-transform infrared spectroscopic analysis of EP showed that the addition of BP significantly inhibited the release of pyrolysis products in the gas phase. The modes of action for flame-retardant BPs in gas phase and condensed phase were proposed.Keywords:few-layer black phosphorus;flame retardant;epoxy resin

研究领域: 材料科学 · 化学工程
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Materials · 2020 ·Vol. 13 ·期 16 ·3550 · IF 3.057

An Extremely Efficient Silylated Benzensulfonate Flame Retardant for Polycarbonate

Xiaodong Lu,Qiang Yao,Weihong Cao,Tianbo Tang

An extremely efficient flame retardant with low water solubility has been developed for bisphenol-A based polycarbonate. Potassium trimethylsilylbenzenesulfonate (KTSS) combining trimethylsilyl and sulfonate groups in its molecule is 7 times less water soluble and 5 times more effective in flame retardancy than potassium benzenesulfonylbenzenesulfonate (KSS), the commercial workhorse for polycarbonate (PC). At a loading of 0.02%, KTSS enables PC to achieve a solid UL-94 V0 rating and a limiting oxygen index (LOI) value of 34.4%, representing an increase of 8.5 units. The extremely high efficiency of KTSS stems from its great migration ability to the burning polymer surface facilitated by trimethylsilyl group, its timely release of active alkaline species that promote the charring process of PC, and the stabilization of char by silicon. In addition to the exceptional flame retardancy, PC/KTSS retains excellent physical properties of PC.Keywords:polycarbonate;flame retardant;sulfonate salts;silicon

CAS / MDL: 13183-70-5 1310-58-3
研究领域: 材料科学 · 化学工程
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Polymers · 2020 ·Vol. 12 ·期 10 ·2407 · IF 3.426

Effect of a Novel Flame Retardant on the Mechanical, Thermal and Combustion Properties of Poly(Lactic Acid)

Mingjun Niu,Zhongzhou Zhang,Zizhen Wei,Wanjie Wang

Poly(lactic) acid (PLA) is one of the most promising biobased materials, but its inherent flammability limits its applications. A novel flame retardant hexa-(DOPO-hydroxymethylphenoxy-dihydroxybiphenyl)-cyclotriphosphazene (HABP-DOPO) for PLA was prepared by bonding 9,10-dihydro-9-oxy-10-phosphaphenanthrene-10-oxide (DOPO) to cyclotriphosphazene. The morphologies, mechanical properties, thermal stability and burning behaviors of PLA/HABP-DOPO blends were investigated using a scanning electron microscope (SEM), a universal mechanical testing machine, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), limiting oxygen index (LOI), vertical burning (UL-94) and a cone calorimeter test (CCT). The LOI value reached 28.5% and UL-94 could pass V-0 for the PLA blend containing 25 wt% HABP-DOPO. A significant improvement in fire retardant performance was observed for PLA/HABP-DOPO blends. PLA/HABP-DOPO blends exhibited balanced mechanical properties. The flame retardant mechanism of PLA/HABP-DOPO blends was evaluated.Keywords:flame retardant;poly(lactic acid);mechanical properties;blends

研究领域: 材料科学 · 燃烧学
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JOURNAL OF APPLIED POLYMER SCIENCE · 2022 ·Vol. 140 ·期 9 ·e53567 · IF 3.057

Flame retardancy, smoke suppression and enhancement properties of Enteromorpha based flame retardants on EPDM

Licong Jiang,Ziwen Zhou,Feng Zhao,Song Li,Zhihua Liu,Xiaoyang Liu,Meiming Xu,Zhenxiang Xin,Shuai Zhao,Lin Li

Enteromorpha as a waste from marine pollution brings great pressure to environmental governance every year, especially for China. Under the premise of shortage of industrial materials, taking appropriate measures can turn waste into wealth, which will benefit us a lot. In this work, a bio-based reinforcing type flame retardant based on Enteromorpha is designed. The designed Enteromorpha based flame retardant system mainly is focused on the reinforcing action and the flame retardant effects on ethylene-propylene-diene tripolymer (EPDM) systemically. Therefore, with the emergence of innovate reinforcing type Enteromorpha flame retardants in the future, the application of Enteromorpha in the polymer flame retardants field will surely usher in bright development.

CAS / MDL: 1401-55-4
研究领域: 材料科学 · 环境科学 · 聚合物工程
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Fire-Switzerland · 2023 ·Vol. 6 ·期 1 ·14 · IF 3.2

Synthesis of High-Efficiency, Eco-Friendly, and Synergistic Flame Retardant for Epoxy Resin

Jiaxiang Gao,Hanguang Wu,Yang Xiao,Wenjing Ma,Fei Xu,Rui Wang,Zhiguo Zhu

It remains a challenge to prepare flame-retardant composites via the addition of a low content of flame retardant. In this work, a novel DOPO-functionalized reduced graphene oxide hybrid (DOPO-M-rGO) flame-retardant system was synthesized for epoxy resin (EP). The phosphorus-nitrogen-reduced graphene oxide ternary synergistic effect provided DOPO-M-rGO with high flame-resistance efficiency in EP; thus, the EP-based composite exhibited superior fire-resistant performance at extremely low DOPO-M-rGO loading. The limiting oxygen index (LOI) of the EP-based composite was increased from 25% to 32% with only 1.5 wt% DOPO-M-rGO addition, and the peak heat release rate (pHRR), total heat release (THR), and total smoke production (TSP) were significantly decreased by 55%, 30%, and 20%, respectively. In addition, as a halogen-free flame-retardant system, DOPO-M-rGO presents great application potential as an eco-friendly additive for the flame-resistance improvement of thermosetting polymer materials.Keywords:flame retardant;epoxy resin;synergistic effect;high efficiency

CAS / MDL: 78-67-1 35948-25-5
研究领域: 材料科学 · 化学工程
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