JOURNAL OF THERMAL ANALYSIS AND CALORIMETRY
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2024
·
IF 3
Tang Gang,Hu Yang,Fang Yuan,Guan Mengfan,Gong Zedong,Wang Guodong,Deng Dan,Liu Xiuyu
A tris(DOPO-grafted piperazine)-triazine phosphoramide (DOPO-TPT) was synthesized, and its structure was well characterized by Fourier transform infrared spectroscopy and nuclear magnetic resonance spectroscopy. DOPO-TPT was used as a flame retardant additive to modify the epoxy resin to obtain a series of flame retardant epoxy thermosets. The effects of DOPO-TPT on the thermomechanical properties, thermal stability and flame retardancy of the resulting epoxy thermosets were investigated. The results showed that when the addition of DOPO-TPT was 5 mass% (phosphorus content was 0.47 mass%), the limiting oxygen index of the epoxy thermoset reached 30.0%, and it passed the UL-94 V-0 classification. Compared with unmodified epoxy resin, the maximum heat release rate and total heat release of EP/DOPO-TPT-5.0 decreased by 28% and 20%, respectively. Additionally, the presence of DOPO-TPT did not deteriorate the thermomechanical properties of the resulting epoxy thermosets. TG-FTIR test confirmed that the incorporation of DOPO-TPT could significantly inhibit the release of gaseous products. The char layer analysis results showed that DOPO-TPT had good catalytic charring performance, which was conducive to decreasing the escape of combustible gas during combustion, thus improving the flame retardancy.
研究领域:
材料科学
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化学工程
✓ 已验证
产品关联
DOI
高影响因子
POLYMER DEGRADATION AND STABILITY
·
2024
·
IF 6.3
Bohan Liang,Ke Liu,Junming Dai,Wenxing Chen,Wangyang Lu
A polymer-type flame retardant (PFR) based on a 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) derivative was synthesised here to improve the flame retardancy of polyamide 6 (PA6). The chemical structure and thermal property of the PFR were characterised by Fourier-transform infrared (FTIR) spectroscopy, nuclear magnetic resonance spectroscopy, gel permeation chromatography (GPC), thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The PFR and PA6 were melt-blended to obtain a flame-retardant polyamide 6 (FRPA6). Its thermal property, mechanical property and flame retardancy were characterised via TGA, DSC and tensile, impact, vertical burning and limiting oxygen index (LOI) tests. Its flame-retardant mode of action was analysed by scanning electron microscopy, FTIR spectroscopy, cone calorimetry and pyrolysis-gas chromatography-mass spectrometry. The FRPA6 with a phosphorus content of 3000 ppm passed the UL-94 V-0 rating, and the LOI of the FRPA6 with a phosphorous content of 5000 ppm reached 28.8 %. Compared with pure PA6 , the peak heat release rate, total heat release and effective heat of FRPA6–5000 were reduced by 35.4 %, 21.9 % and 26.5 %, respectively. These results indicate that the flame-retardant mode of action of PFR mainly involved the quenching effect of phosphorus-containing radicals in the gas phase.
研究领域:
材料科学
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高分子化学
✓ 已验证
产品关联
DOI
高影响因子
FIRE AND MATERIALS
·
2019
·Vol. 43
·期 6
·685-693
·
IF 1.173
Wenpeng Song,Wang Zhang,Yonggang Li,Huijuan Ma,Tao Lin,Cuifen Lu,Junqi Nie,Guichun Yang,Zuxing Chen
Summary Two kinds of novel silicon-phosphorus linear polymers were synthesized by the hydrosilylation reaction of double-decker-shaped silsesquioxane (DDSQ) and 9,10-dihydro-9-oxa-10- phosphaphenanthrene-10-oxide (DOPO) derivatives and characterized using 1 H NMR, 31 P NMR, and 29 Si NMR. Flame-retardant polycarbonate/acrylonitric-butadiene-styrene (PC/ABS) blends were prepared with different contents of silicon-phosphorus linear polymers. The flame-retardant properties of silicon-phosphorus linear polymers as well as the morphology were investigated in detail by using thermogravimetric analysis (TGA), limiting oxygen index (LOI), (Underwriters Laboratory) UL-94, microscale combustion calorimetry (MCC), and scanning electron microscopy (SEM), respectively. The silicon-phosphorus linear polymers containing DDSQ and DOPO units can synergistically improve the flame retardancy and thermal stability of PC/ABS blends. Flame-retardant polymers with different linkers between DDSQ and phosphate units show comparable effect on the flame retardancy of PC/ABS.
研究领域:
材料科学
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高分子化学
✓ 已验证
产品关联
DOI
高影响因子
CELLULOSE
·
2022
·Vol. 29
·期 12
·6941-6962
·
IF 6.123
Tan Wei,Ren Yuanlin,Guo Yingbin,Liu Yansong,Liu Xiaohui,Qu Hongqiang
A novel DOPO derived multi-claw reactive flame retardant (DMCFR) was designed to improve the flame retardancy of lyocell fabric. The chemical structure of DMCFR was identified by proton nuclear magnetic resonance ( 1 H-NMR) and Fourier transform infrared spectroscopy (FT-IR). The chemical structure and elemental composition of the modified lyocell fabric were investigated by FT-IR and X-ray photoelectron spectroscopy. The vertical burning test, limiting oxygen index (LOI) and cone calorimetry were applied to evaluate the flame retardancy of the original and treated samples. The results showed that the peak heat release rate and total heat release of the flame retardant lyocell (FR-lyocell) were significantly reduced by 90.6% and 65.5% compared to control sample. In addition, the LOI value of FR-lyocell fabric was up to 33% and remained 26% even after 20 laundering cycles (LCs). The thermal stability and char-forming capacity of the samples were measured by thermogravimetric analysis, and the residual char of the treated sample was as high as 9.15% and 42.5% under air and nitrogen atmosphere respectively, which were much higher than that of the original sample. Furthermore, the flame retardant mechanism was evidenced via scanning electron microscopy (SEM), Raman spectroscopy, thermogravimetric combined with Fourier transform infrared spectroscopy (TG-IR) and pyrolysis–gas chromatography-mass spectrometry (PyGC-MS), which supported the condensed and gas phase flame retardant mechanism. Graphical abstract
研究领域:
材料科学
·
纺织工程
·
高分子化学
✓ 已验证
产品关联
DOI
高影响因子
POLYMER DEGRADATION AND STABILITY
·
2023
·
IF 5.9
Yifang He,Xinyu Cui,Zhishuo Liu,Fujie Lan,Jun Sun,Hongfei Li,Xiaoyu Gu,Sheng Zhang
Aiming to develop high performance flame-retardant epoxy resin (EP), a novel phosphorus-containing flame retardant named 6-(3-(2-hydroxyphenyl)propyl)dibenzo-[1,2]oxaphosphinine 6-oxide (HP-DOPO) was synthesized and employed as a multi-functional additive for EP with simultaneously excellent flame retardancy, transmittance, mechanical enhancement and anti-aging. With 5 wt.% loading of HP-DOPO, EP composites showed outstanding flame retardancy with a high limiting oxygen index of 35.6 % and V-0 rating in UL-94 test, while the cone calorimetric test results demonstrated that HP-DOPO could efficiently restrain the heat and smoke release. Compared with pure EP, the resultant EP/5 %HP-DOPO exhibited superior mechanical properties with 27.9 % and 56.2 % increase in tensile and impact strengths, respectively. Furthermore, HP-DOPO accelerated the curing procedure and did not sacrifice the transparency of cured EP, while anti-aging performance was obtained at the same time. The exploration of this novel multi-functional additive provided a powerful basis for the technologies and potential industrial applications of epoxy materials.
研究领域:
材料科学
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化学工程
·
高分子科学
✓ 已验证
产品关联
DOI
高影响因子
INDUSTRIAL & ENGINEERING CHEMISTRY RESEARCH
·
2017
·
IF 2.843
Yuan Cao,Xiu-Li Wang,Wen-Qiang Zhang,Xue-Wu Yin,Yue-Quan Shi,Yu-Zhong Wang
A novel reactive phosphorus-containing flame retardant 1,4-phenylene-bis((6-oxido-6H-dibenz[c,e][1,2]-oxaphosphorinyl) methylene) diacrylate (TDCAA-DOPO), with two symmetrical 9,10-dihydro-9-oxa-10-phosphaphena-nthrene-10-oxide structure (bi-DOPO), was synthesized and combined with unsaturated polyester resin (UPR) via cross-linking to prepare flame-retardant UPR (FR-UPR). To make clear both the effects of the bi-DOPO structure and the cross-linking reaction on the thermal stability and flame retardancy of UPR, an additive flame retardant that also owned bi-DOPO structure but without a vinyl bond, 1,4-phenylene-bis((6-oxido-6H-dibenz[c,e][1,2]-oxaphosphorinyl) carbinol) (TDCA-DOPO), was used as a contrast. The results showed that the incorporation of TDCAA-DOPO or TDCA-DOPO into UPR can reduce its peak heat release rate (PHRR) and total heat release (THR), as well as improve the limiting oxygen index (LOI) value. As compared to TDCA-DOPO, the reactive TDCAA-DOPO endowed FR-UPR with enhanced thermal stability, residual char, and glass transition temperature (Tg), which were even higher than those of pure UPR. Besides, their flame-retardant mechanism for UPR had been well investigated.
研究领域:
材料科学
·
高分子化学
✓ 已验证
产品关联
DOI
高影响因子
POLYMERS FOR ADVANCED TECHNOLOGIES
·
2020
·Vol. 32
·期 2
·525-537
·
IF 2.578
Qinqin Luo,Yulin Sun,Biao Yu,Jiangli Song,Dexin Tan,Jianqing Zhao,Shijing Yan
Flame retardants endow epoxy resins (EP) with flame retardance, however, their introduction often lead to the decrease in the glass transition temperature ( T g ), which is an important property for EP. Therefore, it is significant to design and synthesize a high-efficiency flame retardant that enhances flame retardance and T g of EP. To achieve this goal, a hyperbranched polyamide oligomer containing DOPO (HPD) was successfully synthesized by A 4 + B 2 polymerization and its structure was confirmed by FTIR, 1 H NMR, and 30 P NMR spectra and GPC. HPD was used as an additive flame retardant in epoxy resin, and its effect on the flame retardance and thermal properties of epoxy resin was studied. The epoxy resin with 7.5 wt% HPD reached UL-94V-0 rating and a higher LOI value of 29.6%, and its T g was 176.2°C, which is higher than the pure epoxy resin. Moreover, the results of cone calorimetry testing (CCT) and TG-FTIR analysis suggested that the gas-phase and condensed-phase flame-retarded roles of HPD delayed the time to ignition, and reduced the value of relevant combustion parameters, including the peak of heat release rate, average of heat release rate, total heat release, smoke production rate, and total smoke production. The analysis results of Py-GC/MS test of HPD further confirmed that HPD was able to play the flame-retarded role in the gaseous and condensed phases.
研究领域:
材料科学
·
高分子化学
✓ 已验证
产品关联
DOI
高影响因子
POLYMER DEGRADATION AND STABILITY
·
2023
·
IF 5.9
Hu Rong,Yong Guo,Zhongwei Chen,Tingting Chen,Yuan Yu,Chunlei He,Jing Zhou,Xuliang Liu,Qingwu Zhang,Yajie Bu,Juncheng Jiang
A novel reactive flame retardant named PPDA was synthesized by neutralizing phenyl phosphate (PPOA) with 4,4′-diamino diphenyl ether (ODA). When 2.5 wt% of PPDA was incorporated into epoxy resin (EP) alongside 2.5 wt% of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), EP/PPDA/DOPO composite possessed UL-94 V-0 rating and a limited oxygen index (LOI) of 34.2% while exhibiting a remarkable synergistic effect between PPDA and DOPO. In contrast to pure EP, EP/PPDA2.5/DOPO2.5 exhibited a significant reduction in peak heat release rate, total heat release, and total smoke production by 56.3%, 23.0%, and 26%, respectively, when increasing char yield to 30.2%. The synergistic system formed char with organic phosphorus structures containing P-O-C, P-N-C, and P = O bonds, along with benzene rings in the condensed phase, meanwhile forming P-containing radicals and non-flammable nitrogen-containing compounds in the gas stage. Additionally, it was discovered that the presence of the N H bond in PPDA and the P-H bond in DOPO facilitated the ring-opening reaction of the epoxy groups, which contributed to the preservation of the mechanical properties and transparency of the EP. PPDA/DOPO was a halogen-free, low-cost alternative for flame retardants, demonstrating excellent performance and potential for future applications.
研究领域:
材料科学
·
化学工程
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF APPLIED POLYMER SCIENCE
·
2025
·
IF 2.8
Li Tian,Ronghua Chen,Jiang Tan,Fan zhang,Junhong Guo,Bo Mu
To enhance the flame retardancy and smoke suppression performance of epoxy resins (EP), this study reports the synthesis of a high-efficiency flame retardant (SLDH-Ni-KD) through sequential intercalation modification and surface functionalization of layered double hydroxide (LDH). The optimized design addresses both the flame-retardant efficacy enhancement and the inherent compatibility limitations of LDH in EP matrices. Comprehensive combustion characterization was conducted through thermogravimetric analysis (TGA), cone calorimetry testing (CCT), limiting oxygen index (LOI) determination, and UL-94 vertical burning assessment. The underlying flame-retardant mechanism was systematically investigated using scanning electron microscopy, Raman spectroscopy, and thermogravimetry-infrared spectroscopy analysis of char residues. Experimental results revealed that the synergistic interaction between LDH and DOPO components, combined with the bi-phase catalytic charring effects mediated by magnesium/aluminum ions, enabled the 7% SLDH-Ni-KD/EP composite to achieve exceptional fire safety performance. Specifically, the composite demonstrated an elevated LOI value of 33.8% ± 0.1%, accompanied by substantial reductions in total heat release (THR) and smoke production rate (SPR). Mechanical property assessments identified 5 wt.% SLDH-Ni-KD as the optimal loading for maintaining EP matrix compatibility. This work successfully develops an innovative LDH-based nano-flame-retardant system that integrates high-efficiency fire-retardant and smoke-suppressing functionalities, establishing a novel multielement synergistic strategy for polymer flame retardancy.
研究领域:
高分子科学
·
材料工程
·
消防安全工程
·
纳米技术
·
化学改性
✓ 已验证
产品关联
DOI
高影响因子
POLYMER DEGRADATION AND STABILITY
·
2020
·
IF 4.032
Chanchal Kumar Kundu,Xin Wang,Mohammad Ziaur Rahman,Lei Song,Yuan Hu
A DOPO-based phosphorus compound (DOPA) was synthesized and applied onto the pure and chitosan (CS) modified polyamide 66 (PA66) fabric surfaces via a simple pad-dry-cure method to improve the flame retardant properties of the same. The pure and chitosan modified fabric samples treated with DOPA at different content % degraded in a different way as the char residue formation and releasing of volatile and non-volatile gas species were dissimilar which were evident from the thermogravimatric and thermogravimetric-gas chromatography-mass spectroscopy (TG-GC-MS) test analysis. Obtained results also showed that no dripping occurred in the vertical burning test and a sharp increase in limiting oxygen index (LOI) values was noticed for all the treated fabric samples. CS modified PA66 fabric sample treated with a 10 wt % of DOPA exhibited a greater reduction in pHRR by 40% and showed superior flame retardant performance compared to the only DOPA treated pure fabric sample. The superb flame retardant properties of CS modified fabrics were due to the co-presence of DOPA and CS; where a synchronized gas phase and a condensed phase flame retardant mechanism was realized as DOPA showed a quenching effect in a gas phase mechanism and simultaneously, catalyzed the charring of CS in a condensed phase activity which was also justified from the TG-GC-MS analysis, TGA and FTIR analysis of char residues. However, this kind of facile application showed poor wash durability and deteriorated the physical properties of the fabric materials specifically treated with a higher DOPA content.
研究领域:
材料科学
·
纺织工程
·
高分子化学
✓ 已验证
产品关联
DOI
高影响因子
PROGRESS IN ORGANIC COATINGS
·
2025
·
IF 7.3
Ke Wang,Wei Gao
A novel silica-based composite aerogel SA-DKH was synthesized via functionalization of alkali-treated halloysite nanotubes (HNTs-OH) with a DOPO (10-dihydro-9-oxa-10-phospha-phenanthrene-10-oxide)-derived silane coupling agent. SA-DKH exhibited exceptional thermal stability and high specific surface area (748.53–779.62 m 2 /g). In air atmosphere, SA-DKH3 demonstrated a 219.0 °C increase in initial decomposition temperature compared to SA-HNTs3 (composite aerogel synesis using 6 g 4.5 % HNTs-EtOH suspension). SA-DKH significantly enhanced thermal insulation, smoke suppression, and flame retardancy when incorporated into silicone resin composites. Notably, the total smoke production (TSP) of SSDKH4 (composite resin with 8 % SA-DKH) was reduced by 12.2 % (3.90 m 2 ) relative to SSHNTs4 (composite resin with 8 % SA-HNTs). Furthermore, SSDKH4 displayed ultralow thermal conductivity (0.10 W/m·K) and minimal water absorption (0.32 %), while maintaining robust resistance to acids, alkalis, and stains after 12 months of aging. The synergistic flame retardant mechanism involving gas-phase radical quenching by PO·/PO 2 · and condensed-phase char reinforcement via DOPO-HNTs interactions was systematically elucidated. This work provides a novel strategy for designing flame retardant and thermal insulation silicone resin composites.
研究领域:
材料科学
·
化学工程
✓ 已验证
产品关联
DOI
高影响因子
SURFACE & COATINGS TECHNOLOGY
·
2024
·
IF 5.3
Xiaokang Zhang,Li Zhang,Jing Chen,Xiangzhan Jiang,Yu Wei,Fei Xiao,Jinghui Hu,Jiawang Ding
Facing the escalating issue of industrial wastewater discharge and its profound environmental repercussions, the creation of novel sponge materials that excel in oil-water separation while incorporating flame retardancy becomes critically urgent. Despite their superior absorption capabilities, conventional oil-water separation sponges typically overlook flame retardant features, a limitation that curtails their applicability. To address this gap, we have developed a multifunctional hydrophobic sponge through a sophisticated multi-step chemical self-assembly process. This method grafts 9,10-Dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and perfluorinated compounds onto melamine foam (MF), yielding a composite material designated as DOPO-PF@MF. DOPO-PF@MF boasts a dual functionality of hydrophobicity and flame retardance. Its modified surface exhibits a pronounced hydrophobic-lipophilic balance, with a static water contact angle of 134°. It also displays favorable wetting characteristics towards various organic solvents, such as methanol, ethanol, dimethylformamide, dichloromethane, and hexane. This material demonstrates an impressive adsorption capacity for these solvents, with the adsorption-desorption capacity for ethanol remaining consistent over ten cycles. Furthermore, DOPO-PF@MF efficiently separates emulsions of methylene chloride and water, showcasing its versatility. Moreover, DOPO-PF@MF exhibits commendable chemical resilience under extreme temperatures, ranging from 0 °C to 100 °C, and withstands both acidic and alkaline conditions (pH 1–14), preserving its structural integrity against corrosive substances. Most notably, it surpasses unmodified melamine foam in flame retardancy. The incorporation of DOPO fortifies the material's resistance to high-temperature ignition, effectively inhibiting flame propagation and reducing burn rate, enhancing safety measures.
研究领域:
材料科学
·
环境科学
✓ 已验证
产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）