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Synthesis of Organic-Inorganic Hybrid Aluminum Hypophosphite Microspheres Flame Retardant and Its Flame Retardant Research on thermoplastic polyurethane

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Journal of Wuhan University of Technology(Materials Science) 2024年第1期39卷 221-233页

作者：刘生鹏 XU Zhi ZHANG Xinyuan WEI Huan XIONG Yun DING Yigang HUANG Wenbo 许莉莉 Engineering Research Center of Phosphorus Resources Development and Utilization of Ministry of Education Key Laboratory for Green Chemical Process of Ministry of EducationSchool of Chemical Engineering and PharmacyWuhan Institute of TechnologyWuhan 430205China Hubei Three Gorges Laboratory Yichang 443007China School of Technology Materials Science and Engineering Wuhan Institute of TechnologyWuhan 430205China

Aluminum hypophosphite microspheres(AHP) were synthesized by hydrothermal method using NaH2PO2·H2O and AlCl3·6H2O as raw materials, and then the AHP microspheres were polymerized by surface polymerization of micro-nanospheres with cyclic cross-linked poly(cyclotriphosphazene-co-4,4'-sulfonyldiphenol)(PZS). A new organic-inorganic poly(phosphonitrile)-modified aluminum hypophosphite microspheres(PZS-AHP) were synthesized by encapsulation and applied to flame retardant thermoplastic polyurethane(TPU). The microstructure and chemical composition of the PZS-AHP microsphere were characterized by scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy and X-ray spectroscopy. The thermal stability of PZS-AHP microsphere was explored with thermogravimetric analysis. Thermogravimetric data indicate that the PZS-AHP microspheres have excellent thermal stability. The thermal and flame-retarding properties of the TPU composites were evaluated by thermogravimetric(TG), limited oxygen index tests(LOI), and cone calorimeter test(CCT). The TPU composite achieved vertical burning(UL-94) V-0 grade and LOI value reached 29.2% when 10 wt% PZS-AHP was incorporated. Compared with those of pure TPU, the peak heat release rate(pHRR) and total heat release(THR) of TPU/10%PZS-AHP decreased by 82.2% and 42.5%, respectively. The results of CCT indicated that PZS-AHP microsphere could improve the flame retardancy of TPU composites.

关键词： polyphosphazene thermoplastic polyurethane flame retardancy aluminum hypophosphite surface polymerization

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Surface decoration of Halloysite nanotubes with POSS for fire-safe thermoplastic polyurethane nanocomposites

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Journal of Materials Science & Technology 2022年第6期101卷 107-117页

作者： Wei Wu Wanjing Zhao Xianjing Gong Qijun Sun Xianwu Cao Yujun Su Bin Yu Robert K.Y.Li Roy A.L.Vellaisamy Department of Materials Science and Engineering City University of Hong KongTat Chee AvenueKowloonHong Kong SARChina National Engineering Research Center of Novel Equipment for Polymer Processing Key Laboratory of Polymer Processing Engineering of Ministry of EducationGuangdong Provincial Key Laboratory of Technique and Equipment for Macromolecular Advanced ManufacturingSchool of Mechanical and Automotive EngineeringSouth China University of TechnologyGuangzhou 510640China National-certified Enterprise Technology Center Kingfa Science and Technology Co.Ltd.Guangzhou 510663China Centre for Future Materials University of Southern QueenslandToowoombaQueenslandAustralia James Watt School of Engineering University of GlasgowGlasgow G128QQUnited Kingdom

Halloysite nanotubes(HNTs)have been considered as a promising flame retardant fillers for *** this work,the polyhedral oligomericsilsesquioxane(POSS)containing amino group was covalently grafted on the surface of HNTs with 3-(2,3-epoxypropoxy)propytrimethoxysilane as a chemical *** POSS modified HNTs(HNTs-POSS)dispersed uniformly in the thermoplastic polyurethane(TPU)matrix and endowed TPU nanocomposites with enhanced tensile properties and fire *** calorimeter tests revealed that the introduction of 2 wt%HNTs-POSS to TPU matrix remarkably reduced the peak of heat release rate(PHRR)and total heat release(THR)by 60.0%and 18.3%,*** addition,the peak CO production rate and total smoke release(TSR)could be significantly suppressed by the addition of *** well dispersed HNTs in combination with the ceramified silicon network from the thermal decomposition of POSS contributed to the formation of a continuous and compact char layer,exhibiting a tortuous effect by inhibiting heat diffusion and evaporation of volatile *** addition,the released crystal water from HNTs could dilute the combustible volatiles and then decline the combustion *** tensile tests demonstrated that introduction of 2 wt%HNTs-POSS would enhance the maximum stress of TPU nanocomposite with a slight decrease of elongation at *** combination of HNTs and POSS through the construction of effective interfacial interactions provides a feasible way to effectively enhance the fire safety of TPU nanocomposites without scarifying ductility.

关键词： thermoplastic polyurethane Halloysite nanotube POSS Flame retardancy Mechanical property

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Temperature-induced Evolution of Micro-structure and Chain Dynamics in thermoplastic polyurethane with Low Hard Segment Content as Studied by In Situ Synchrotron SAXS and Time-Domain NMR Experiments

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Chinese Journal of Polymer Science 2023年第12期41卷 1902-1911,I0008页

作者： Hong-Ru Wang Victor Litvinov Wei Yu Kar Wee Eddie Peh Qian-Li Yu Yong-Feng Men State Key Laboratory of Polymer Physics and Chemistry Changchun Institute of Applied ChemistryChinese Academy of SciencesChangchun 130022China School of Applied Chemistry and Engineering University of Science and Technology of ChinaHefei 230026China BASF polyurethane Specialties(China)Co.Ltd. Shanghai 200137China V.Lit.Consult Gozewijnstraat 46191 WV Beekthe Netherlands

The microstructural evolution of a thermoplastic polyurethane(TPU)with low hard segment content has been monitored utilizing in situ real-time synchrotron small angle X-ray scattering(SAXS)and time-domain nuclear magnetic resonance(NMR)*** TPU is composed of 23 wt% of[4,4-methylenediphenyl diisocyanate(MDI)]-[1,4-butanediol(BD)]chain segments,which form hard domains,as[polytetrahydrofuran(PTHF)]forming soft *** number and distribution of monomer units in hard blocks is determined by the successive self-nucleation and annealing thermal fractionation *** situ SAXS method reveals heating-induced increase in the spacing of hard and soft domains,while time-domain ^(1)H-NMR characterizes the changes in the phase composition and chain dynamics in these domains.A glassy fraction of short MDI-BD chain segments in hard domains passes through T_(g) above ambient *** higher temperatures,MDI-BD nanocrystals start to *** length distribution of MDI-BD chain segments causes a distribution in crystal sizes and wide melting temperature *** melting is accompanied by the mixing of MDI-BD with PTHF segments in soft domains,and by increase in segmental mobility in these *** 180℃,the TPU melt is homogeneous on the scale above nanometers according to SAXS data.

关键词： Phase separation thermoplastic polyurethane Melting behavior Time-domain NMR SAXS

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Smoke suppressant in flame retarded thermoplastic polyurethane composites: Synergistic effect and mechanism study

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Nano Research 2021年第11期14卷 3926-3934页

作者： Hongyuan Ren Kelan Qing Ying Chen Yanjun Lin Xue Duan State Key Laboratory of Chemical Resource Engineering Beijing University of Chemical TechnologyBeijing100029China

Considerable smoke and toxic volatiles generation has compromised the application of thermoplastic polyurethane (TPU) and caused a great threat to human life. Here, nano-MgFe layered double hydroxide (MgFe-LDH) with uniform particle size was synthesized to reduce smoke density and toxic gases of TPU composites using ammonium polyphosphate (APP) as a flame retardant agent. The results show that the combination of 16 wt.% APP and 4 wt.% MgFe-LDH greatly decreased the smoke density (D20min and Ds, max), smoke production rate (SPR) and heat release rate (HRR) of TPU composites. Furthermore, the MgFe-LDH synergist demonstrated high efficiency in decreasing total volatiled products and toxic volatiles evolved, such as the CO, HCN and isocyanates. The reason was mainly attributed to the chemical reaction between MgFe-LDH and APP, which can promote the compactness of char layers with fine microstructure formed in the decomposition process of MgFe-LDH/APP/TPU composites. The protective char layers could act as barriers between combustion zone and matrix to protect the unburned substrate and promote smoke suppression effect.

关键词： layered double hydroxide thermoplastic polyurethane smoke suppression synergistic effect

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Dynamic Bonds Mediate π-π Interaction via Phase Locking Effect for Enhanced Heat Resistant thermoplastic polyurethane

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Chinese Journal of Polymer Science 2021年第2期39卷 154-163,I0005页

作者： Yue Lai Xiao Kuang Wen-Hong Yang Yu Wang Ping Zhu Jing-Pu Li Xia Dong Du-Jin Wang CAS Key Laboratory of Engineering Plastics CAS Research/Education Center for Excellence in Molecular SciencesInstitute of ChemistryChinese Academy of SciencesBeijing 100190China University of Chinese Academy of Sciences Beijing 100049China The George W.Woodruff School of Mechanical Engineering Georgia Institute of TechnologyAtlantaGeorgia 30332United States College of Materials Science and Engineering Shenzhen UniversityShenzhen 518060China

Stimulus-responsive polymers containing dynamic bonds enable fascinating properties of self-healing,recycling and reprocessing due to enhanced relaxation of polymer chain/network with labile ***,we study the structure and properties of a new type of thermoplastic polyurethanes(TPUs)with trapped dynamic covalent bonds in the hard-phase domain and report the frustrated relaxation of TPUs containing weak dynamic bond andπ-πinteraction in hard *** detected by rheometry,the aromatic TPUs with alkyl disulfide in the hard segments possess the maximum network relaxation time in contrast to those without dynamic bonds and alicyclic *** situ FTIR and small-angle scattering results reveal that the alkyl disulfide facilitates stronger intermolecular interaction and more stable micro-phase morphology inπ-πinteraction based aromatic *** dynamics simulation for pure hard segments of model molecules verify that the presence of disulfide bonds leads to strongerπ-πstacking of aromatic rings due to both enhanced assembling thermodynamics and *** enhancedπ-πpacking and micro-phase structure in TPUs further kinetically immobilize the dynamic *** kinetically interlocking between the weak dynamic bonds and strong molecular interaction in hard segments leads to much slower network relaxation of *** work provides a new insight in tuning the network relaxation and heat resistance as well as molecular self-assembly in stimulus-responsive dynamic polymers by both molecular design and micro-phase control toward the functional applications of advanced materials.

关键词： thermoplastic polyurethane Disulfide bond Stimuli-responsive rearrangement π-πStacking Phase locked effect

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Effect of LiTFSI and LiFSI on Cycling Performance of Lithium Metal Batteries Using thermoplastic polyurethane/Halloysite Nanotubes Solid Electrolyte

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Acta Metallurgica Sinica(English Letters) 2021年第3期34卷 359-372页

作者： Zhichuan Shen Jiawei Zhong Wenhao Xle Jinbiao Chen Xi Ke Jianmin Ma Zhicong Shi School of Materials and Energy Guangdong University of TechnologyGuangzhou 510006China Guangdong Engineering Technology Research Center for New Energy Materials and Devices Guangzhou 510006China School of Physics and Electronics Hunan UniversityChangsha 410082China

All-solid-state lithium batteries(ASSLB) are promising candidates for next-generation energy storage ***,the large-scale commercial application of high energy density AS S LB with the polymer electrolyte still faces *** this study,a thin solid polymer composite electrolyte(SPCE) is prepared through a facile and cost-effective strategy with an infiltration of thermoplastic polyurethane(TPU),lithium salt(LiTFSI or LiFSI),and halloysite nanotubes(HNTs) in a porous framework of polyethylene separator(PE)(TPU-HNTs-LiTFSI-PE or TPU-HNTs-LiFSI-PE).The composition,electrochemical performance,and especially the effect of anions(TFSI-and FSI-) on cycling performance are *** results reveal that the flexible TPU-HNTs-LiTFSI-PE and TPU-HNTs-LiFSI-PE with a thickness of 34 μm exhibit wide electrochemical windows of 4.9 and 5.1 V(***+/Li) at 60℃,*** in FSI-tends to form more LiF and sulfur compounds at the interface between TPU-HNTs-LiFSI-PE and Li metal anode,thus enhancing the interfacial *** a result,cell composed of TPU-HNTs-LiFSI-PE exhibits a smaller increase in interfacial resistance of solid electrolyte interphase(SEI) with a distinct decrease in charge-transfer resistance during ***|Li symmetric cell with TPU-HNTs-LiFSI-PE could keep its stable overpotential profile for nearly 1300 h with a low hysteresis of approximately39 mV at a current density of 0.1 mA cm-2,while a sudden voltage rise with internal cell impedance-surge signals was observed within 600 h for cell composed of *** initial capacities of NCMITPU-HNTs-LiTFSIPEILi and NCMITPU-HNTs-LiFSI-PEILi cells were 149 and 114 mAh g-1,with capacity retention rates of 83.52% and89.99% after 300 cycles at 0.5 C,*** study provides a valuable guideline for designing flexible SPCE,which shows great application prospect in the practice of ASSLB.

关键词： Solid polymer composite electrolyte Lithium metal anode thermoplastic polyurethane Halloysite nanotubes Cycling performance

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Antibacterial thermoplastic polyurethane/PL-DOSS Composite Films

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Chinese Journal of Polymer Science 2021年第8期39卷 1020-1028,I0007页

作者： Xiao Liu Jian-Wei Guo Ya-Dong Liu Ming Liu Hui Liu Miao-Miao Han Sheng-Xiang Ji Key Laboratory of Polymer Ecomaterials Changchun Institute of Applied ChemistryChinese Academy of SciencesChangchun 130022China School of Applied Chemistry and Engineering University of Science and Technology of ChinaHefei 230026China

Medical devices-related infections pose a great threat to patients and cause an increased morbidity and mortality. Herein, we prepare an antibacterial composite(TPU-x) through blending medical grade thermoplastic polyurethane(TPU) and the complex(PL-DOSS) of ε-polylysine(ε-PL) and docusate sodium(DOSS). >99% reduction of colony forming unit(CFU) can be obtained in TPU-x composite films even at relatively low content of PL-DOSS, e.g. 0.13% for Methicillin resistant S. aureus(MRSA) and 0.5% for E. coli. The excellent antibacterial activity is mainly attributed to the formation of PL-DOSS nanoparticles that are uniformly dispersed in the TPU matrix with a size of ~100 nm. TPU-x composite films exhibit long-term stability in saline and good biocompatibility, and retain mechanical properties of TPU.

关键词： Nosocomial infections Antibacterial composite Solution blending thermoplastic polyurethane Polylysine

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MORPHOLOGY AND PERFORMANCE OF UNSATURATED POLYESTER NANOCOMPOSITES MODIFIED WITH ORGANOCLAY AND thermoplastic polyurethane

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Chinese Journal of Polymer Science 2010年第6期28卷 913-922页

作者： Chang-jiang You Jin-guo Xua Yi-zheng Zeng Yao Li De-min Jia Toshio Nishi College of Materials Science and Engineering South China University of Technology Guangzhou 510640 China WPI Advanced Institute for Materials Research Tohoku University 2-1-1 Katahira Aoba Sendai 980-8577 Japan

Unsaturated polyester（UPR）/thermoplastic polyurethane（TPU）/organoclay nanocomposites were prepared by melt compounding of thermoplastic polyurethane and unsaturated polyester prepolymer,and then mixing with the hybrids of styrene monomers and organoclay at ambient *** crosslinking reaction eventually occurred through the unsaturated polyester prepolymer and styrene *** morphology of the composites was investigated by scanning electron microscopy（SEM） and transmission electron microscopy（TEM）.The results show that the impact strength of UPR/TPU/organoclay nanocomposites increases obviously;the cure shrinkage decreases markedly,the glass transition temperature is enhanced and an elastic response to the deformation is prominent at the temperature above 10℃.

关键词： Unsaturated polyester thermoplastic polyurethane Organoclay Nanocomposites

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Microcellular injection molding process for producing lightweight thermoplastic polyurethane with customizable properties

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Frontiers of Mechanical Engineering 2018年第1期13卷 96-106页

作者： Thomas ELLINGHAM Hrishikesh KHARBAS Mihai MANITIU Guenter SCHOLZ Lih-Sheng TURNG Department of Mechanical Engineering University of Wisconsin-Madison Madison WI 53706 USA Wisconsin Institute for Discovery University of Wiseonsin-MadisonMadison WI 53715 USA BASF Corporation Wyandotte MI 48192 USA

A three-stage molding process involving microcellular injection molding with core retraction and an ＂out-of-mold＂ expansion was developed to manufacture thermoplastic polyurethane into lightweight foams of varying local densities, microstructures, and mechanical properties in the same microcellular injection molded part. Two stages of cavity expansion through sequential core retractions and a third expansion in a separate mold at an elevated temperature were carried out. The densities varied from 0.25 to 0.42 g/cm3 （77% to 62% weight reduction）. The mechanical properties varied as well Cyclic com- pressive strengths and hysteresis loss ratios, together with the microstructures, were characterized and reported.

关键词： thermoplastic polyurethane microcellularinjection molding cavity expansion compressive strength,hysteresis loss ratio

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Improving the Compatibility of Biodegradable Poly (Lactic Acid) Toughening with thermoplastic polyurethane (TPU) and Compatibilized Meltblown Nonwoven

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Open Journal of Composite Materials 2022年第1期12卷 1-15页

作者： Md Obaidur Rahman Feichao Zhu Bin Yu College of Textile Science and Engineering Zhejiang Provincial Key Laboratory of Industrial Textile Materials and Manufacturing Technology Zhejiang Sci-Tech University Hangzhou China

Poly (Lactic Acid) (PLA) is a biodegradable polymer which originates from natural resources such as corn and starch, offering excellent strength, biodegradability, nevertheless its inherent brittleness and low impact resistance properties have limited its application. On the other hand, Thermoplastic Polyurethane (TPU) has high toughness, durability and flexibility, which is one of the most potential alternatives for enhancing the flexibility and mechanical strength of Poly (Lactic Acid) (PLA) by blending it with a compatibilizer. With the aim to improve the mechanical and thermal properties of

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