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JOURNAL OF APPLIED POLYMER SCIENCE · 2024 ·Vol. 142 ·期 2 ·e56359 · IF 2.7

Lignin-based nitrogen and phosphorus-containing polylactic acid with flame-retardant performances

Guixin Zhang,Shuxian Weng,Jie Wang,Zhimin Kou,Meiting Liu,Guoqiang Zhu,Lihong Hu,Yonghong Zhou

Polylactic acid (PLA) is a new type of biodegradable material that has been applied in many fields such as extrusion, injection molding, film drawing, and spinning. In contrary, it does not have flame retardancy. In this paper, N-PCDL was synthesized by amidation reaction between  COOH of PCDL and  NH 2 of tetraethylenepentamine (TEPA), followed by an Atherton-Todd reaction of unreacted  NH 2 at the other end of TEPA with P  H of DOPO to prepare a novel lignin-based flame retardant containing nitrogen and phosphorus (NP-PCDL). The Fourier transform infrared spectroscopy (FT-IR) and nuclear magnetic hydrogen spectroscopy ( 1 H NMR) analysis results showed that proton peaks of  CO  NH  , P  N  , and  NH  appeared in the NP-PCDL spectrum, while the characteristic absorption peak of P  H bond disappeared in DOPO, the X-ray photoelectron spectroscopy (XPS) results showed that the degraded lignin consisted of elements C and O, while NP-PCDL consisted of elements C, O, N and P. The above results indicated that NP-PCDL was successfully prepared. NP-PCDL accounted for 3% (mass percentage, the same below), 5% and 10% of PLA, then lignin based flame-retardant PLA composites were prepared by internal mixing and injection molding. Thermogravimetric analysis (TGA) showed that the residual carbon of PLA/3% NP-PCDL, PLA/5% NP-PCDL and PLA/10% NP-PCDL at 800°C were higher than that of pure PLA, with the increase of 56.56%, 97.54%, and 301.64%, respectively; The analysis of SEM, XPS, and Raman showed that PLA/NP-PCDL formed dense, regular and highly graphitized residual carbon with phosphorus nitrogen structure during the combustion process. At the same time, NH 3 , H 2 O and PO˙ free radicals were released, which could dilute combustible gases, destroy free radical chain reaction, isolate combustible gases and heat, so as to play a flame-retardant role.

CAS / MDL: 6066-82-6
研究领域: 材料科学 · 化学工程
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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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CELLULOSE · 2019 ·Vol. 26 ·期 11 ·6995-7007 · IF 3.917

Solvent-free synthesis of silicon–nitrogen–phosphorus flame retardant for cotton fabrics

Tian Peixiu,Lu Yi,Wang Dingfei,Zhang Guangxian,Zhang Fengxiu

Abstract Combustible cotton fabric has limited applications particularly as a flame retardant. In this study, an efficient flame retardant ammonium of aminopropyl silanol methylene phosphate (AASMP) was synthesized using 3-aminopropylethoxysilane, phosphorous acid, urea and formaldehyde under mild and solvent-free conditions to solve cotton inflammable problems. AASMP was grafted onto the surface of cotton fabric, and new P–O–C covalent bonds, were generated using pad-curing treatment to obtain flame-retardant cotton fabrics. The treated cotton was characterized by scanning electron microscopy/energy-dispersive spectroscopy, Fourier-transform infrared spectroscopy and X-ray diffraction, and confirmed that AASMP was grafted well with slight damage to the cotton structure. Cotton treated with 30% AASMP achieved a 45.0% high limiting oxygen index (LOI). After 50 laundering cycles, a 31.0% LOI was retained, indicating that AASMP imparted remarkable flame retardancy and excellent washing durability to cotton. The results of cone calorimetry showed that the peak-heat release rate of the treated cotton was 6.57 kW/m 2 , which was significantly lower than that of the control cotton (186.55 kW/m 2 ). Thermogravimetric results demonstrated that treated cotton with 34.2 wt% residue at 800 °C exhibited significant thermal stability and thermal oxidation stability. The mechanical property of the treated cotton slightly decreased but retained more than 70%. Treated cotton can be used in clothing and interior items. Graphic abstract

CAS / MDL: 919-30-2
研究领域: 材料科学 · 纺织工程 · 燃烧化学
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JOURNAL OF APPLIED POLYMER SCIENCE · 2025 · IF 2.8

The Synergistic Effect of Ammonium Polyphosphate and a N/P/Si-Containing Intumescent Flame Retardant on the Flame-Retardant Properties of Polylactic Acid

Feijing Xu,Nian Yin,Shanjun Gao,Chunhui Shen

Ammonium polyphosphate (APP) and intumescent flame-retardant di-(3-amin-opropyltriethoxysilane) spirocyclic pentaerythritol diphosphate (PDAP) were prepared as an intumescent flame retardant with synergistic effect, and polylactic acid (PLA) was modified by melt blending. The flame retardancy of PLA/PDAP/APP was evaluated by limiting oxygen index (LOI), vertical combustion test (UL-94), and cone calorimetry test (CCT), and the thermal stability of PLA/PDAP/APP was studied by thermogravimetric analysis and thermogravimetry-Fourier transform infrared spectroscopy (FTIR). The possible flame-retardant mechanisms of PLA/PDAP/APP were analyzed based on the results of laser Raman spectroscopy and FTIR. When PDAP:APP = 2:1 and the addition amount of PDAP/APP is 20 wt%, the LOI value of PLA/IFR-modified material is as high as 43%, and the UL-94 test reaches V-0 level, and in the CCT, the PHRR and THR of PLA/PDAP/APP (2:1)-modified material are reduced by 80.7% and 76.8%, respectively, compared with pure PLA, and the carbon residue is as high as 62.01%. The results show that the compound APP/PDAP has an excellent flame-retardant effect on PLA, which provides a good research case for PLA flame-retardant-modified plastic materials.

研究领域: 材料科学 · 高分子化学
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Materials Today · 2025 · IF 22

Exceptional flame-retardant, super strong/tough, and superhydrophobic/self-cleaning wood

Feng Gu,Xianhao He,Youhang Wei,Xiuxue Niu,Zhaosheng Cai,Bo Jiang,J.Y. Zhu,Wangxia Wang

This study presents a novel approach to fabricate wood composites with exceptional flame retardancy, superior strength and toughness, as well as superhydrophobic/self-cleaning properties. The fabrication process involves densifying delignified wood pre-impregnated with a nitrogen-phosphorus flame retardant via hot-pressing, followed by an adhesive-free, self-curing superhydrophobic dip-coating. The resulting wood exhibits remarkable synergistic performance: exceptional flame retardancy, with peak heat release rate (pHRR) and total heat release (THR) decreased by 77.7 % and 63.6 %, respectively, compared with pristine wood; superhydrophobicity/self-cleaning with a water contact angle (WCA) of 161.2° and sliding rolling off angle (SA) of 3.9°; and outstanding mechanical performance with a tensile strength of 439 MPa and fracture toughness of 8.7 MJ/m 3 . Notably, this innovation addresses two critical challenges in fire-retardant wood technology—preventing flame retardant leaching and eliminating flammable adhesives—thereby offering a scalable method for the commercial production of high-performance wood composites suitable for applications in green architecture, transportation, and safety–critical infrastructure.

研究领域: 材料科学 · 阻燃技术 · 木材科学 · 表面工程 · 复合材料
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