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1.
The synergistic effect of 9,10‐dihydro‐9‐oxa‐10‐phosphaphenanthrene‐10‐oxide (DOPO) immobilized silica (SiO2‐DOPO) nanoparticles with an intumescent flame retardant (IFR) on the flame retardancy of polypropylene (PP) was investigated by UL 94 vertical tests and limiting oxygen index (LOI) measurements. It was found that the PP/IFR composites (25 wt%) achieved the UL94 V0 grade and LOI increased to 32.1 with an incorporation of 1.0 wt% SiO2‐DOPO nanoparticles. Based on thermogravimetric analysis, scanning electronic microscopy and rheological analysis, it is speculated that three factors are mainly contributed to the improvement of the flame retardancy. First, the thermal stability of PP/IFR composites was improved by incorporating SiO2‐DOPO nanoparticles. Second, the presence of SiO2‐DOPO nanoparticles could induce the formation of a continuous char skin layer during combustion. The compact char layer could effectively impede the transport of bubbles and heat. Third, rheological analysis indicated that SiO2‐DOPO nanoparticles could increase viscosity of the PP/IFR composites, which was also benefited to increase flame retardancy. Copyright © 2013 John Wiley & Sons, Ltd.  相似文献   

2.
The charring agent (CNCA‐DA) containing triazine and benzene rings was combined with ammonium polyphosphate (APP) to form intumescent flame retardant (IFR), and it was occupied to modify polylactide (PLA). The flame retardant properties and mechanism of flame retardant PLA composites were investigated by the limited oxygen index (LOI), vertical burning test (UL‐94), thermogravimetric analysis, microscale combustion calorimetry, scanning electron microscopy, laser Raman spectroscopy analysis and X‐ray photoelectron spectroscopy. The analysis from LOI and UL‐94 presented that the IFR was very effective in flame retardancy of PLA. When the weight ratio of APP to CNCA‐DA was 3:1, and the IFR loading was 30%, the IFR showed the best effect, and the LOI value reached 45.6%. It was found that when 20 wt% IFR was loaded, the flame retardancy of PLA/IFR still passed UL‐94 V‐0 rating, and its LOI value reached 32.8%. The microscale combustion calorimetry results showed that PLA/IFR had lower heat release rate, total heat release, and heat release capacity than other composites, and there was an obvious synergistic effect between APP and CNCA‐DA for PLA. IFR containing APP/CNCA‐DA had good thermal stability and char‐forming ability with the char residue 29.3% at 800°C under N2 atmosphere. Scanning electron microscopy observation further indicated that IFR could promote forming continuous and compact intumescent char layer. The laser Raman spectroscopy analysis and X‐ray photoelectron spectroscopy analysis results indicated that an appropriate graphitization degree of the residue char was formed, and more O and N were remained to form more cross‐linking structure. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

3.
The functions of nanoclay and three different boron containing substances, zinc borate (ZnB), borophosphate (BPO4), and boron silicon containing preceramic oligomer (BSi), were studied to improve the flame retardancy of polypropylene (PP)‐nanoclay‐intumescent system composed of ammonium polyphosphate (APP) and pentaerythritol (PER). The flame retardancy of PP composites was investigated using limiting oxygen index (LOI), UL‐94 standard, thermogravimetric analysis (TGA), and cone calorimeter. According to the results obtained, the addition of 20 wt% intumescent flame retardant (IFR) improved the flame retardancy by increasing the char formation. Addition of clay slightly increases the LOI value and reduces the maximum heat release rate (HRR). Addition of clay also increases the barrier effect due to intumescent char, especially in thin samples. Boron compounds show their highest synergistic effect at about 3 wt% loading. According to UL‐94 test and LOI test, 3 wt% ZnB containing composite shows the highest rating (V0) and BPO4 containing sample shows the highest LOI value (26.5). Copyright © 2010 John Wiley & Sons, Ltd.  相似文献   

4.
In this work, 12‐tungestocobaltic acid based organic–inorganic hybrid material, [Bmim]6CoW12O40 (CoW) was synthesized and applied as a synergist in polypropylene (PP)/intumescent flame retardant (IFR) composites. The flame retardant properties were investigated by the limiting oxygen index (LOI), UL‐94 vertical burning test, thermal gravimetric analyzer (TGA), cone calorimeter and scanning electron microscopy (SEM) etc. The results showed that the PP composites with 16 wt% IFR and 1 wt% CoW achieves the UL‐94 V‐0 rating and gets a LOI value 28.0. However, only add no less than 25 wt% single IFR, can the PP composites obtain the UL‐94 V‐0 rating, which suggests that CoW has good synergistic effects on flame retardancy of PP/IFR composites. In addition, the SEM and cone calorimeter tests indicated the CoW improves the quality of char layer. The rate of char formation has been enhanced also because of the existence of CoW. It is the combination of a better char quality and a high rate of char formation promoted by CoW that results in the excellent flame retardancy of PP/IFR composites. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

5.
Flame‐retardant polyamide 6 (PA6) was prepared by an inorganic‐organic composite (MCN or MgO/g‐C3N4) synthesized by incorporating magnesium oxide (MgO) combined with graphitic carbon nitride (g‐C3N4). As compared to g‐C3N4, MCN possessed a laminate structure, more holes, and a larger specific surface area. The addition of MCN could effectively improve the flame retardancy and mechanical properties of PA6 due to its better compatibility and dispersion in the PA6 matrix. When the addition of MCN was 20 wt%, the vertical combustion performance of the PA6/MCN sample reached flammability rating V‐0 (UL‐94) and the limiting oxygen index (LOI) was up to 32.1%. The results of thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) revealed that the introduction of MCN efficiently enhanced thermal stability of PA6. The morphologies of the char residue observed by scanning electron microscopy (SEM) verified that MCN promoted the formation of sufficient, compact, and homogeneous char layers on the composite's surface during burning. Thus led to increase the char layer strength and improve the flame retardancy of PA6. The thermogravimetric analysis/infrared (TG‐IR) revealed the gas‐phase retardancy mechanism of MCN. Compared with PA6/g‐C3N4, PA6/MCN showed better mechanical properties in terms of flexural strength and tensile strength.  相似文献   

6.
The synergistic effect of four different boron containing substances, zinc borate (ZnB), borophosphate (BPO4), boron silicon containing preceramic oligomer (BSi) and lanthanum borate (LaB), were studied to improve the flame retardancy of a polypropylene (PP) intumescent system composed of ammonium polyphosphate (APP) and pentaerythritol (PER). The flame retardancy of PP composites was investigated by limiting oxygen index (LOI), UL-94 standard, thermogravimetric analysis (TGA) and cone calorimeter tests. The addition of 20 wt% intumescent flame retardant (IFR) improves the flame retardancy by increasing the char formation. According to LOI and UL-94 test, boron compounds show their highest synergistic effect at 1 wt% loading. BPO4 containing composite shows the highest LOI (30), lowest maximum heat release rate (HRR) and lowest total heat release rate (THR) value. Although the char yield increases as the amount of boron compounds increases, the flame retarding effect decreases. Cone calorimeter and TGA data indicate that the boron compounds are likely to show their synergistic effect by reinforcing the integrity of char which improves its barrier effect rather than increasing the char yield.  相似文献   

7.
Herein, a bridged 9,10‐dihydro‐9‐oxa‐10‐phosphaphenanthrene‐10‐oxide (DOPO) derivative (PN‐DOPO) in combination with organ‐montmorillonite (OMMT) was used to improve the flame retardancy and mechanical properties of glass‐fiber‐reinforced polyamide 6 T (GFPA6T). The flame retardancy and thermal stabilities of the cured GFPA6T composites were investigated using limiting oxygen index, vertical burning (UL‐94) test, cone calorimeter test, and thermogravimetric analysis (TGA). The morphological analysis and chemical composition of the char residues after cone calorimeter tests were characterized via scanning electron microscopy and energy dispersive spectrometry. The results indicate that 2 wt% OMMT combined with 13 wt% PN‐DOPO in GFPA6T achieved a V‐0 rating in UL‐94 test. The peak heat release rate and total smoke release remarkably decreased with the incorporation of OMMT as compared to those of GFPA6T/15 wt% PN‐DOPO. The TGA results show that the thermal stability and residual mass of the samples effectively increased with the increase in OMMT content. The morphological analysis and composition structure of the residues demonstrate that a small amount of OMMT could help form a more thermally stable and compact char layer during combustion. Also, with the incorporation of OMMT, the layers consisted of more carbon‐silicon and aluminum phosphate char in the condensed phase. Furthermore, GFPA6T/PN‐DOPO/OMMT composites exhibited excellent mechanical properties in terms of flexural modulus, flexural strength, and impact strength than the GFPA6T/PN‐DOPO system. The combination of PN‐DOPO and OMMT has improved the flame retardancy and smoke suppression of GFPA6T without compromising the mechanical properties.  相似文献   

8.
Aluminum hypophosphite (AHP) was introduced into polylactide/intumescent flame retardant (PLA/IFR) systems by melt blending. The flame retardant and thermal properties of the PLA composites were investigated. The results suggest that a synergistic effect exists between IFR and AHP on the char formation and anti‐dripping behavior of PLA composites. The PLA/IFR composites containing 10 wt% IFR can pass the UL‐94 V‐0 rating but the test is accompanied by heavy melt dripping. For the PLA/AHP a UL‐94 V‐2 rating is obtained for the same loading of IFR. However, the composites containing 7 wt% IFR and 3 wt% AHP pass the UL‐94 V‐0 rating with modified dripping behavior. Moreover, the char from combustion of PLA/IFR is flexible but of poor quality. That for PLA/AHP is brittle with many cracks. In contrast, that for PLA/IFR/AHP is strong and compact. Thus it can resist the erosion due to heat and gas formation and protect the inside of the matrix. In addition, AHP causes the crosslinking among APP, which promotes the char formation and prevents the melt dripping. This is the main reason for the good flame retardant properties of PLA composites. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

9.
Molybdenum trioxide (MoO3) microrods, nanofibers, and nanoplates were synthesized via the hydrothermal method and high‐temperature calcination method, respectively. Then the MoO3 was added into polyurethane elastomer, respectively. The flame retardancy and smoke suppression of the composites added with different MoO3 were studied by thermal gravimetric analysis, cone calorimeter, and smoke density. The results show that the three kinds of MoO3 with different morphologies could promote the formation of char and possess flame retardancy and smoke suppression, and MoO3 nanofibers exhibit a higher degree of flame retardancy, and 1 wt% addition could make the peak heat release rate of polyurethane elastomer composites reduce from 881.6 kW m?2 for a pure sample to 343.4 kW m?2, a decrease by 61.0%. As for smoke suppression, MoO3 nanoplates possess the best smoke suppression; 5 wt% could decrease a pure sample's smoke density by 41.3% from 361 to 212. Moreover, the char residue of composites after combustion was analyzed by Raman spectra and X‐ray photoelectron spectroscopy, and the flame retardancy and smoke suppression mechanisms of MoO3 were discussed.  相似文献   

10.
The flame‐retardant polylactic acid (PLA) has been prepared via mixing the flame retardant TGIC‐DOPO derived from phosphaphenanthrene and triazine groups into matrix. The flame retardancy of TGIC‐DOPO/PLA composites was characterized using the limiting oxygen index (LOI), vertical burning test (UL94), and cone calorimeter test. Results reveal that the 10%TGIC‐DOPO/PLA composite obtained 26.1% of LOI and passed UL94 V‐0 rating. The flame‐retardant mechanism of PLA composites was characterized via thermogravimetric analysis (TGA), pyrolysis gas chromatography/mass spectroscopy, and TGA‐Fourier transform infrared. It discloses that TGIC‐DOPO promoted PLA decomposing and dripping early, and it also released the fragments with quenching and dilution effects. These actions of TGIC‐DOPO contribute to reducing the burning intensity and extinguishing the fire on droplets, thus imposing better flame retardancy to PLA. When TGIC‐DOPO was partly replaced by melamine cyanuric with dilution effect and hexa‐phenoxy‐cyclotriphosphazene with quenching effect in composites respectively, the results confirm that TGIC‐DOPO utilize well‐combination in dilution effect and quenching effect to flame retard PLA. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

11.
DOPO and boron nitride (BN) fillers with different particle sizes and several loadings were employed to improve the properties of cyanate ester (CE) resin. The effects of BN content and particle size on the thermal conductivity of the BN‐DOPO/CE ternary composites were discussed. The influence of enhancing the thermal conductivity of the ternary composites on their flame retardancy was studied. The consequences showed that increasing the thermal conductivity of BN‐DOPO/CE composites had an active impact on their flame retardancy. Approving flame retardancy of the ternary composites was certified by the high limiting oxygen index (LOI), UL‐94 rating of V‐0, and low heat release rate (HRR) and total heat release (THR). For instance, in contrast with pure CE matrix, peak of HRR (pk‐HRR), average of HRR (av‐HRR), THR, and average of effective heat of combustion (av‐EHC) of CEP/BN0.5 μm/10 composite were decreased by 51.7%, 33.8%, 18.7%, and 18.9%, respectively. Thermal gravimetry analysis (TGA) showed that the addition of BN fillers improves the thermal stability of the composites. Moreover, the ternary composites possess good dielectric properties. Their dielectric constants (ε) are less than 3, and dielectric loss tangent (tgδ) values are lower than neat CE resin.  相似文献   

12.
The effects of lanthanum oxide (La2O3) as a synergistic agent on the flame retardancy of intumescent flame retardant polypropylene composites (IFR-PP) were studied, and the new IFR system mainly consisted of the charring-foaming agent (CFA) and ammonium polyphosphate (APP). The limiting oxygen index (LOI), UL-94 test, thermogravimetric analysis (TGA), cone calorimeter (CONE) and scanning electron microscopy (SEM) were used to evaluate the synergistic effects of La2O3. It was found that when IFR was fixed at 20 wt% in IFR-PP composites, only a little amount of La2O3 could enhance LOI value and pass the UL-94 V0 rating test (1.6 mm). The TGA data showed that La2O3 could enhance the thermal stability of the IFR-PP systems at high temperature and effectively increase the char residue formation. The CONE results revealed that La2O3 and IFR could clearly change the decomposition behavior of PP and form a char layer on the surface of the composites, consequently resulting in efficient reduction of the flammability parameters, such as heat release rate (HRR), total heat release (THR), smoke production rate (SPR), total smoke production (TSP), ignition time (IT) and so on. The morphological structures observed by SEM demonstrated that La2O3 could promote to form the homogenous and compact intumescent char layer. Thus, a suitable amount of La2O3 plays a synergistic effect in the flame retardancy and smoke suppression of IFR composites.  相似文献   

13.
A phosphorus and silicon containing liquid monomer (9,10‐dihydro‐9‐oxa‐10‐phosphaphenanthrene 10‐oxide–vinyltrimethoxysilane (DOPO–VTS)) was synthesized by the reaction between DOPO and VTS. DOPO–VTS and methacryloxypropyltrimethoxylsilane were introduced into unsaturated polyester resin to prepare flame retardant UPR/SiO2 (FR‐UPR/SiO2) hybrid materials by sol–gel method and curing process. DOPO–VTS contributes excellent flame retardancy to UPR matrix, which was confirmed by the limiting oxygen index and microscale combustion calorimeter results. The thermogravimetric analysis (TGA) results indicate that the FR‐UPR/SiO2 hybrid materials possess higher thermal stability and residual char yields than those of pure UPR at high temperature region. The thermal degradation of materials was investigated by TGA/infrared spectrometry (TG‐IR) and real‐time infrared spectrometry (RT‐IR), providing insight into the thermal degradation mechanism. Moreover, scanning electron microscopy (SEM) and X‐ray photoelectron spectroscopy (XPS) were used to explore the morphologies and chemical components of the residual char. Copyright © 2013 John Wiley & Sons, Ltd.  相似文献   

14.
Establishing a phosphorus‐free strategy to fabricate high‐performance thermosetting resins owning outstanding thermal resistance, good flame retardancy, and smoke suppression is important for sustainable development. Herein, a unique phosphorus‐free hybrid (BN@CeO2) was synthesized through chemically grafting cerium oxide (CeO2) on surface of exfoliated boron nitride (BN) nanosheet with the aids of γ‐aminopropyltriethoxysilane and polydopamine coating, which was then embedded into bisphenol A cyanate ester (BCy) resin to fabricate new BN@CeO2/BCy composites with high thermal resistance. Compared with BCy resin, the BN@CeO2/BCy composite with 4 wt% BN@CeO2 not only has delayed initial ignition time by 23 seconds but also severally shows 58.1%, 23.1%, and 44.4% lower smoke produce rate, total heat release, and peak heat release rate. The study on mechanism behind outstanding flame retardancy reveals that the improved heat resistance and flame retardancy of BN@CeO2/BCy composite are attributed to multiply effects induced by BN@CeO2 and its interaction with BCy resin; specifically, these effects come from BN (physical barrier) and CeO2 (free radical trapping effect and catalytic char layer formation) as well as those from the synergistic effect of BN and CeO2. These excellent comprehensive properties of BN@CeO2/BCy composites demonstrate that BN@CeO2 is an environment‐friendly and synergistic modifier for developing heat‐resisting thermosetting resins with outstanding flame retardancy and smoke suppression.  相似文献   

15.
A novel activated carbon spheres (ACS)@SnO2@NiO hierarchical hybrid architecture was first synthesized and applied for enhancing the flame retardancy of epoxy (EP) resin via a cooperative effect. Herein, using activated carbon microspheres as the template, SnO2 and NiO nanospheres were successively anchored to it by a sedimentation‐calcination strategy. The well‐designed ACS@SnO2@NiO significantly enhanced the flame retardancy for consistency of EP composites, as demonstrated by thermogravimetric and cone calorimeter experiments. For instance, the incorporation of 2 wt% ACS@SnO2@NiO decreased by 15.5% maximum in the total smoke production, accompanying the higher graphitized char layer. In addition, the synergetic mechanism of flame retardancy between ACS@SnO2@NiO and aluminum hypophosphite (AHP) was investigated. The obtained sample satisfied the UL‐94 V‐0 rating with a 5.0 wt% addition of AHP and ACS@SnO2@NiO (the ratio of the mass fraction of AHP to ACS@SnO2@NiO is 4.5:0.5). Notably, the incorporation of AHP and ACS@SnO2@NiO resulted in a significant decrease in the fire hazard properties of EP resin; for instance, 4.5AHP‐0.5ACS@SnO2@NiO/EP resulted in a maximum decrease of 32.4% in the total smoke production as compared with that of pure EP resin. It should be noted that the improved flame‐retardant performance for the EP composites is primarily attributed to the synergistic effect of ACS@SnO2@NiO and AHP in promoting the formation of residual char in the condensed phase.  相似文献   

16.
Ammonium polyphosphate (APP) and inorganic fillers were applied for improving flame retardancy and mechanical performance of recycled poly(ethylene terephthalate) (RPET). RPET was compounded with 5–10 wt% of talc and glass bead using twin screw extruder then were injection molded with 2 wt% of APP. The effects of fillers contents and APP on properties and flame retardancy of RPET composites were investigated. The incorporation of talc and glass bead as well as the adding of APP significantly improved tensile and flexural modulus of RPET composites. Scanning electron microscope micrographs indicated good distribution of talc, while glass bead was agglomerated on the RPET matrix. Flame‐retardant property of neat RPET and the RPET composites revealed V‐2 of UL‐94 flammability rating. It can be noted that the composites were less dripping because of the synergistic effect of adding talc and glass bead with APP. From thermogravimetric analysis results, larger of residual char contents and lower values of the activation energy were considered for enhancing flame retardancy in the RPET composites. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

17.
The effects of β‐cyclodextrin containing silicone oligomer(CDS), as a synergistic agent, on the flame retardancy and mechanical properties of intumescent flame retardant polypropylene composites were studied by adding different amounts of CDS in intumescent flame retardants. The limiting oxygen index (LOI), UL‐94 test, thermogravimetric analysis (TGA), and scanning electron microscopy (SEM) were utilized to evaluate the synergistic effects of CDS in the composites. It was found that after a little amount of CDS partially replaced a charring‐foaming agent (CFA) in IFR, LOI values of the composites were enhanced and they obtained a UL‐94 V‐0 rating. IFR system containing 6.25wt% CDS presented the best flame retardancy in PP. The experimental results obtained from LOI and UL‐94, TGA, SEM, and mechanical properties indicated that the combination of CDS and CFA presents synergistic effects in flame retardancy, char formation, and mechanical properties of the composites. This is probably due to different structures of polyhydroxyl macromolecules (CDS and CFA), the existence of dimethyl silicone group in CDS, and the toughness of epoxy silicon chain in CDS. SEM results proved that the interfacial compatibility between IFR and PP was improved by CDS. Copyright © 2009 John Wiley & Sons, Ltd.  相似文献   

18.
An intumescent flame retardant spirocyclic pentaerythritol bisphosphorate disphosphoryl melamine (SPDPM) has been synthesized and its structure was characterized by Fourier transformed infrared spectrometry (FTIR), 1H and 31P nuclear magnetic resonances (NMR). A series of polylactide (PLA)-based flame retardant composites containing SPDPM were prepared by melt blending method. The combustion properties of PLA/SPDPM composites were evaluated through UL-94, limiting oxygen index (LOI) tests and microscale combustion calorimetry (MCC) experiments. It is found that SPDPM integrating acid, char and gas sources significantly improved the flame retardancy and anti-dripping performance of PLA. When 25 wt% flame retardant was added, the composites achieved UL-94 V0, and the LOI value was increased to 38. Thermogravimetric analysis (TGA) showed that the weight loss rate of PLA was decreased by introduction of SPDPM. In addition, the thermal degradation process and possible flame retardant mechanism of PLA composites with SPDPM were analyzed by in situ FTIR.  相似文献   

19.
To develop environmental‐friendly and flame‐retarded polymer composites, bio‐based polylactic acid (PLA) was loaded with thermally stable polyhedral octaphenyl silsesquioxane (OPS). Pure PLA and PLA/OPS composites with the OPS of 1, 3, 5, and 10 wt% were prepared by extrusion and injection molding, respectively. The scanning electron microscopy (SEM), polarized optical microscope (POM), differential scanning calorimetry (DSC), X‐ray diffraction (XRD), and thermal gravimetric analysis (TGA) were used to analyze the dispersion of the OPS in the PLA matrix and the effects of OPS on the crystallization and thermal stability properties of PLA/OPS composites, respectively. Limited oxygen index (LOI) and cone calorimeter (CONE) measurements were used to study flame retardancy of PLA and PLA/OPS composites. In order to study the flame‐retardant mechanism, the char residues were investigated by SEM, Fourier transform infrared spectra (FTIR), and X‐ray photoelectron spectroscopy (XPS). TGA‐FTIR was used to analyze the gaseous products of their thermal decomposition. The results show that the OPS particles were submicron in the PLA and could increase the crystallization rate of PLA and form small‐sized secondary α‐form crystalline compared with the pure PLA spherulite. The PLA and OPS decomposed individually in the PLA/OPS composites by TGA. According to the LOI tests, the PLA with the OPS loading exhibited very small reduction of LOI. However, the CONE tests indicated that the OPS could improve the flame retardancy of the PLA by means of low peak heat release rate and average heat release rate. It was obtained that the degree and type of the PLA crystalline for the pure PLA and PLA/OPS affect their flame retardancy. In the max thermal decomposition stage of PLA and PLA/OPS, their gaseous products were similar; at high temperatures, the PLA/OPS produced simple and clear gaseous products of PLA with solid SiO2 in the gas phase.  相似文献   

20.
A novel hyperbranched polyamine charring agent (HPCA), a derivative of triazines, was synthesized and well characterized by 1H NMR and FTIR. HPCA and ammonium polyphosphate (APP) were added into polylactide (PLA) resin as an intumescent flame retardant (IFR) system to impart flame retardancy and dripping resistance to PLA. The flammability and thermal stability of IFR-PLA composites were investigated by limiting oxygen index (LOI), UL-94 vertical burning, cone calorimetry and thermogravometric analysis (TGA) tests. The results showed that the IFR system had both excellent flame retardant and anti-dripping abilities for PLA. The TGA curves suggested that HPCA has good ability of char formation and when combined with APP, would induce synergistic effect which could be clearly observed. This effect greatly promoted the char formation of IFR-PLA composites, hence improved the flame retardant property. Additionally, the structure and morphology of char residues were studied by XPS, FTIR and SEM.  相似文献   

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