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Chinese Journal of Structural Chemistry 2017年第7期36卷 1117-1123页

作者：马小平黄钰天郑寅王东华王军刚宋新建 Hubei Key Laboratory of Biological Resources Protection and Utilization Hubei University for Nationalities School of Chemical and Environmental Engineering Hubei University for Nationalities

The title compound, 2-（3-silatranylpropylamino）-4-dichlorophenyl-5,5-dimethyl- 1,3,2-dioxaphosphorinane-2-oxide （2（C20H33N2O6Psi）？C2H6O？CH4O, Mr = 991.20）, has been synthe- sized by the nucleophilic substitution reaction of 2-chloro-4-phenyl-5,5-dimethyl-1,3,2-dioxa- phosphorinane-2-oxide with γ-aminopropylsilatrane, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P with a = 10.3783（15）, b = 11.2402（17）, c = 12.1675（18）？, ？ = 70.653（4）, ？ = 82.908（4）, ？ = 85.690（4）？, V = 1328.1（3）？3, Z = 1, Dc = 1.239 g/cm3, μ = 0.19 mm？1, F（000） = 532, the final R = 0.0640 and wR = 0.2090 for 3615 observed reflections with I 〉 2？（I）. The cyclic dioxaphosphorinane ring in the molecule adopts a thermodynamically stable cis conformation, while the silatrane fragment forms a cage-like structure in which there exists an intramolecular Si？N donor-acceptor bond. In the crystal structure, centrosymmetrically related molecules are linked by pairs of N–H？？？O hydrogen bonds into dimers, generating rings with graph-set motif R22（8）. Furthermore, a couple of O（7）–H（10）？？？O（3） hydrogen bonds were formed by O atom of P=O and H atom from hydroxyl in the solvent ethanol. Thermal property of the compound was also studied by means of thermogravimetry （TGA）. The thermal analysis and preliminary fireproofing test show that the title compound has good flame retardance.

关键词： 1,3,2-dioxaphosphorinane-2-oxide crystal structure epoxy resin flame retardance

Thermal Runaway of Lithium-Ion Batteries Employing flame-Retardant Fluorinated Electrolytes

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Energy & Environmental Materials 2023年第1期6卷 333-339页

作者： Junxian Hou Li Wang Xuning Feng Junpei Terada Languang Lu Shigeaki Yamazaki Anyu Su Yoshiko Kuwajima Yongjiang Chen Tomoya Hidaka Xiangming He Hewu Wang Minggao Ouyang State Key Laboratory of Automotive Safety and Energy Tsinghua UniversityBeijing 100084China Institute of Nuclear and New Energy Technology Tsinghua UniversityBeijing 100084China Daikin Industries Ltd.1-1Nishi-HitotsuyaSettsu Osaka 566-8585Japan Sichuan New Energy Vehicle Innovation Center Yibin 644002China

Fluorinated electrolytes possess good antioxidant capacity that provides high compatibility to high-voltage cathode and flame retardance;thus,they are considered as a promising solution for advanced lithium-ion batteries carrying both high-energy density and high safety.Moreover,the fluorinated electrolytes are widely used to form stable electrolyte interphase,due to their chemical reactivity with lithiated graphite or lithium.However,the influence of this reactivity on the thermal safety of batteries is seldom discussed.Herein,we demonstrate that the flame-retardant fluorinated electrolytes help to reduce the flammability,while the lithium-ion batteries with flame-retardant fluorinated electrolytes still undergo thermal runaway and disclose their different thermal runaway pathway from that of battery with conventional electrolyte.The reduction in fluorinated components(e.g.,LiPF 6 and fluoroethylene carbonate(FEC))by fully lithiated graphite accounts for a significant heat release during battery thermal runaway.The 13%of total heat is sufficient to trigger the chain reactions during battery thermal runaway.This study deepens the understanding of the thermal runaway mechanism of lithium-ion batteries employing flame-retardant fluorinated electrolytes,providing guidance on the concept of electrolyte design for safer lithium-ion batteries.

关键词： battery safety flame retardance fluorinated electrolytes lithium-ion battery thermal runaway

Minimizing Carbon Content with Three-in-One Functionalized Nano Conductive Ceramics:Toward More Practical and Safer S Cathodes of Li-S Cells

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Energy & Environmental Materials 2023年第3期6卷 31-39页

作者： Ning Li Chang Sun Jianhui Zhu Shun Li Yanlong Wang Maowen Xu Changming Li Jian Jiang School of Materials and Energy and Chongqing Key Lab for Advanced Materials and Clean Energies of TechnologiesSouthwest UniversityChongqing 400715China School of Physical Science and Technology Southwest UniversityChongqing 400715China Key Laboratory of Chemical Lasers Dalian Institute of Chemical PhysicsChinese Academy of SciencesDalian 116023China College of Chemistry and Chemical Engineering Key Laboratory of Laser Technology and Optoelectronic Functional Materials of Hainan Provinceand Key Laboratory of Functional Materials and Photoelectrochemistry of HaikouHainan Normal UniversityHaikou 571158China

Using porous carbon hosts in cathodes of Li-S cells can disperse S actives and offset their poor electrical conductivity.However,such reservoirs would in turn absorb excess electrolyte solvents to S-unfilled regions,causing the electrolyte overconsumption,specific energy decline,and even safety hazards for battery devices.To build better cathodes,we propose to substitute carbons by In-doped SnO_(2)(ITO)nano ceramics that own three-in-one functionalities:1)using conductive ITO enables minimizing the total carbon content to an extremely low mass ratio(~3%)in cathodes,elevating the electrode tap density and averting the electrolyte overuse;2)polar ITO nanoclusters can serve as robust anchors toward Li polysulfide(LiPS)by electrostatic adsorption or chemical bond interactions;3)they offer catalysis centers for liquid–solid phase conversions of S-based actives.Also,such ceramics are intrinsically nonflammable,preventing S cathodes away from thermal runaway or explosion.These merits entail our configured cathodes with high tap density(1.54 g cm^(−3)),less electrolyte usage,good security for flame retardance,and decent Li-storage behaviors.With lean and LiNO_(3)-free electrolyte,packed full cells exhibit excellent redox kinetics,suppressed LiPS shuttling,and excellent cyclability.This may trigger great research enthusiasm in rational design of low-carbon and safer S cathodes.

关键词： flame retardance Li-S cells minimized carbon ratio nano conductive ceramics three-in-one functionality

Blow spinning mass production of melamine@polyacrylonitrile composite nanofibers with enhanced flame-retardant and strengths

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Progress in Natural Science:Materials International 2023年第5期33卷 634-643页

作者： Jiahao He Wenlu Zhang Xinpeng Jin Chong He Wenbin Li School of Textile Science and Engineering Wuhan Textile University State Key Laboratory of New Textile Materials and Advanced Processing Technologies Wuhan Textile University

To achieve the scalable production of high-performance melamine-based flame retardant nanofibers, solution blowing spinning technology was employed into the continuous spinning of melamine(MA)@polyacrylonitrile(PAN) composite fibers. Propelled by the compressed air current, spinnable MA@PAN solutions can be shaped into nanofiber with a high flow rate over 50 m L/h. Among different melamine-based materials,melamine phosphate(MPP) exhibited excellent solubility in the solution, exceeding 30 wt%, ensuring that the MPP@PAN nanofiber products demonstrated exceptionally robust flame-retardant performance. Furthermore,through fiber textile needle punching technology, loose fiber sponge can be organized into enhanced fiber blankets. These MPP@PAN nanofiber products exhibited outstanding flame retardant and thermal insulation properties, rendering them pivotal as the flame-retardant materials in extreme environments.

关键词： Composites flame retardance High temperature materials Mechanical properties Nanofibers

A Study on a Magnesium-Based Layered Composite Used as a flame Retardant for Phenolic Epoxy Resins

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Fluid Dynamics & Materials Processing 2022年第3期18卷 549-561页

作者： Hongxiang Liu Neng Xiong Songli Wang Wei Zhang Bo Yong National Engineering Laboratory for Vacuum Metallurgy Key Laboratory of Nonferrous Metals Vacuum Metallurgy of Yunnan ProvinceKunming650093China Faculty of Metallurgical and Energy Engineering Kunming University of Science and TechnologyKunming650093China

The effects of a magnesium-based layered composite on the flammability of a phenolic epoxy resin(EP)are studied.In order to produce the required composite material,first,magnesium hydroxide,aluminum salt and deionized water are mixed into a reactor according to a certain proportion to induce a hydrothermal reaction;then,the feed liquid is filtered out using a solid-liquid separation procedure;finally,the material is dried and crushed.In order to evaluate its effects on the flammability of the EP,first,m-phenylenediamine is added to EP and vacuum defoamation is performed;then,EP is poured into a polytetrafluoroethylene mold,cooled to room temperature and demoulded;finally,the magnesium-based layered composite is added to EP,and its flame retardance is characterized by thermogravimetric analysis,limiting oxygen index and cone calorimetry.The X-ray diffraction patterns show that the baseline of magnesium-based layered composite is stable and the front shape is sharp and symmetrical when the molar ratio of magnesium to aluminium is 3.2:1;with the addition of magnesium-based layered composite,the initial pyrolysis temperature of EP of 10%,15%and 30%magnesium-based layered composite decreases to 318.2°C,317.9°C and 357.1°C,respectively.After the reaction,the amount of residual carbon increases to 0.1%,3.45%and 8.3%,and the limiting oxygen index increases by 28.3%,29.1%and 29.6%,respectively.The maximum heat release rate of cone calorimeter decreases gradually.The optimum molar ratio of Mg:Al for green synthesis is 3.2:1,and the NO_(3)-intercalated magnesium-based layered composite has the best flame retardance properties.

关键词： Phenolic epoxy resin layered composite green synthesis flame retardance anion intercalation

SYNERGISTIC EFFECTS OF NOVOLAC-BASED CHAR FORMER WITH A PHOSPHORUS/NITROGEN-CONTAINING flame RETARD ANT IN POLYAMIDE 6

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Chinese Journal of Polymer Science 2012年第1期30卷 72-81页

作者： Wei-cheng Xiong Li Chen De-yi Wang Fei Song Yu-zhong Wang Center for Degradation an-d flame--Retardant Polymeric Materials College of-Chemistry State Key Laboratory of Polymer Materials Engineering National Engineering Laboratory of Eco-Friendly Polymeric Materials （Sichuan） Sichuan University Chengdu 610064 China

The synergistic effect of phosphorus oxynitride（PON） with a novolac-based char former modified by salification （NA-metal salt） on the flame retardance of polyamide 6（PA6） was investigated.For this purpose,various flame-retardant PA6 systems were melt-compounded with PON,PON/NA,PON/NA-V_2O_5 and PON/NA-Fe_2O_3,and their flame retardance was evaluated by measuring the limiting oxygen index（LOI） values and UL-94 vertical burning ratings.The results showed that,compared with the PA6/PON/NA system,the combination of two char formers（NA-V_2O_5,NA-Fe_2O_3） with PON could obviously improve the char formation and flame retardance of PA6.The flame retardance and cone calorimetric analyses showed the stronger synergism as well as the better flame retardant performance of PON/NA-Fe_2O_3 flame retardant system. The effects of different char formers on the flame retardance and thermal stability of this system were also discussed.

关键词： Polyamide flame retardance Novolac resin Synergistic effect

Preparation of Polystyrene/Triphenyl Phosphate Composites by Suspension Polymerization and Melt Extrusion Method A Comparative Study

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Chinese Journal of Polymer Science 2016年第6期34卷 688-696页

作者： Cun-wei Zhang Rong-jie Yang 李向梅 De-qi Yi National Engineering Research Center of flame Retardant Materials School of Materials Beijmg Institute of Technology Beijing 100081 China Fire Command Department Chinese People's Armed Police Forces Academy Langfang 065000 China

Polystyrene （PS）/triphenyl phosphate （TPP） composites were prepared by both suspension polymerization and melt extrusion, and a comparative study of the flame retardance and mechanical properties was carried out. The results showed that suspension polymerization was a better technique than melt extrusion for obtaining good dispersity of the PS/TPP composite. The TPP nanoparticles, which were approximately 50 nm in size, were homogenously and uniformly dispersed in the PS matrix by suspension polymerization in one-step. However, the PS/TPP composite was partially agglomerated, exhibiting irregularly shaped micron-scale particles as a result of melt extrusion. In contrast to the melt extrusion, the limited oxygen index （LOI） of the PS/TPP nanocomposite by suspension polymerization increased to 22.6% from 21.8%, and time to ignition （TTI） increased by 12.3%, the peak heat release rate （PHRR） decreased by 8.5%, and the total heat release （THR） decreased by 11.0%. The mechanical properties of the PS/TPP nanocomposite by suspension polymerization also increased. The tensile strength, elongation at break, and flexural strength increased by 36.4%, 8.5%, and 108%, respectively.

关键词： Polystyrene Triphenyl phosphate flame retardance Suspension polymerization Melt extrusion.

Improved flame resistance properties of unsaturated polyester resin with TiO2-MXOY solid superacid

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Chinese Journal of Chemical Engineering 2020年第9期28卷 2474-2482页

作者： Xuexi Chen Mei Wan Ming Gao Yanxia Wang Deqi Yi School of Safety Engineering North China Institute of Science and TechnologyBeijing 101601China School of Environmental Engineering North China Institute of Science and TechnologyBeijing 101601China National Laboratory of flame Retardant Materials School of Materials Science and EngineeringBeijingInstitute of TechnologyBeijing 100081China

Five SO4^2-/TiO2-MXOY solid super acids(SSA:Cu@Ti:SSA,Zr@Ti:SSA,Fe@Ti:SSA,Mn@Ti:SSA,Mo@Ti:SSA)were successfully prepared by sol-gel method,and its chemical structure and element content were characterized by X-ray diffraction(XRD)analysis,Fourier transform infrared spectroscopy(FHIR)and energy dispersive spectroscopy(EDS).Then,a compound flame retardant system containing SSA and ammonium polyphosphate/montmorillonite(AM)were was introduced into an unsaturated polyester resin(UPR)to enhance the flame retardance.The effect of SSA on the flammability and thermal stability of the UPR was evaluated by the limiting oxygen index(LOI),cone calorimeter te st(CCT)and thermogravimetric analysis(TGA).The LOI results showed that the flame retardance of the UPR composites was significantly improved with the addition of SSA.Moreover,their heat release rate(HRR),total heat release(THR),the smoke production rate(SPR)and CO and CO2 yield were much decreased.In addition,the initial decomposition temperature of UPR/AM/S SA was delayed,indicating that their thermal stability was increased,and the residual char of UPR/AM/SSA was also increa sed due to strong catalytic of SSA ability for esterification and dehydration.Furthermore,the microstructure of the residual char after combustion of the UPR composites was studied by the scanning electron microscopy(SEM),and it was found that the char layer structure was more continuous and dense after the addition of the SSA.In sum up,the synergistic effect between SSA and AM was the main factor for the great improvement of flame retardant of UPR composites.

关键词： flame retardance Unsaturated polyester resin(UPR) Solid super acid Cone calorimeter

STUDIES ON COMBUSTION BEHAVIOR OF NR/MMT NANO-COMPOSITES BY CONE CALORIMETER

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Chinese Journal of Polymer Science 2007年第5期25卷 535-539页

作者：王文涛 College of Material Science and Engineering South China University of Technology

The NR/modified montmorillonite （EMT） nano-composites were prepared by mechanical mixing and reacting in situ with glycidyl methacrylate. Under 30 kW·m^-2 of heat flux, the combustion behavior of the nano-composites was studied with cone calorimetry, and PHRR, THR, EHC, TSR and MLR were tested. The results showed that the nanocomposite had improved mechanical properties and flame retardance properties, and to some extent, the nano-composite had smoke suppress effect. Compared with pure NR, the PHRR, EHC and SPR of the nano-composite reduced by 34%, 21% and 16.8%, respectively.

关键词： NR GMA Modified montmorillonite flame retardance Cone calorimetry.