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1.
A novel flame‐retardant (SPDH) containing phosphorus was synthesized through the reaction of 10‐(2,5‐dihydroxyphenyl)‐9,10‐dihydro‐9‐oxa‐10‐phosphaphenanthrene‐10‐oxide and synthesized intermediate product 3,9‐dichloro‐2,4,8,10‐tetraoxa‐3,9‐diphosphaspiro[5.5] undecane‐3,9‐dioxide, which was used for optimizing the flame retardancy of ethylene‐vinyl acetate copolymer (EVM) rubber/aluminum hydroxide (ATH) composites. The microstructure of SPDH was characterized and determined by Fourier transform infrared and nuclear magnetic resonance spectroscopy. Thermogravimetric analysis (TGA) showed that SPDH had good charring effect at high temperature (600°C). The flame retardancy of the optimized EVM/ATH composites by SPDH was investigated by limiting oxygen index (LOI), cone calorimeter, and UL‐94 vertical burning tests. A higher LOI value (29.8%) and better UL‐94 rating (V‐0) can be achieved for the optimized EVM/ATH composite (EVM‐7) than EVM/ATH composite without SPDH (EVM‐3) with the total loading of additives. The heat release rate decreased and residual mass increased gradually as the loading of SPDH increased for the optimized EVM/ATH composites. There existed distinct synergistic flame‐retardant effect between SPDH and ATH in EVM matrix. POLYM. COMPOS., 2011. © 2011 Society of Plastics Engineers  相似文献   

2.
The effect of percolation and catalysis of bamboo‐based active carbon (BAC) on the thermal degradation and flame retardancy of ethylene vinyl‐acetate rubber (EVM) composites with intumescent flame retardants (IFR) consisting of ammonium polyphosphate (APP) and dipentaerythritol (DPER) has been investigated. The vulcanization characteristics were analyzed by a moving die rheometer. Thermogravimetric analysis (TGA) and fire behavior tests such as limiting oxygen index (LOI), vertical burning (UL 94), and cone calorimetry were used to evaluate the thermal properties and flame retardancy of EVM composites. Scanning electron microscopy (SEM) was used to study the morphology of residues of EVM composites. The addition of BAC significantly increased the maximum torque (MH) of EVM composites and EVM matrices. The combination of IFR with BAC can improve the thermal stability of EVM composites. Moreover, BAC can enhance char residue and promote the formation of a network for IFR. The current EVM/37IFR/3BAC composite achieved an LOI of 33.6% and a UL 94 V‐0 rating. The PHRR, total heat release (THR), and total smoke release (TSR) for EVM/IFR/BAC were greatly reduced as compared to EVM/40IFR. Also, the mechanical properties of the EVMIFR/BAC composites increased with increasing BAC contents. The physical percolation effect between BAC and EVM before and after thermal degradation, and the chemical catalysis effect between BAC and IFR during thermal degradation are responsible for the improved flame retardancy of EVM composites. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42414.  相似文献   

3.
A novel flame retardant (SPDV) containing phosphorus and silicon elements at the same time was synthesized. Spirocyclic pentaerythritol bisphosphorate disphosphoryl chloride (SPDPC) synthesized through simple dehydrochlorination reaction of pentaerythritol (PER) and phosphorus oxychloride (POCl3) was introduced into 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO)/ vinylmethyldimethoxy silane (VMDMS) oligomer (DV) to form a novel flame retardant. The structure and properties of SPDPC, DV and SPDV were characterized by FT-IR, NMR and TGA. After blended with EVM, the flame retardance of EVM/SPDV composites was estimated by cone calorimeter, limited oxygen index (LOI) and UL-94, and thermal stability was investigated using TGA. The morphological structure of the char formed after combustion in cone calorimeter was investigated by Scanning Electron Microscopy (SEM). The results indicate that the flame retardant and thermal stability were improved by incorporation of SPDV. The rich foamed char layers were observed in the residues after combustion in cone calorimeter test, which exactly benefits the thermal stability and flame retardant of EVM materials.  相似文献   

4.
A halogen‐free intumescent flame retardant expandable graphite composite (EG), with an initial expansion temperature of 202°C and expansion volume of 517 mL g−1, was successfully prepared via a facile two‐step intercalation method, i.e. using KMnO4 as oxidant and H2SO4, Na2SiO3·9H2O as intercalators. The prepared EG flame retardant was characterized by field emission scanning electron microscope, X‐ray diffraction spectroscopy, energy dispersive spectroscopy and Fourier transform infrared spectroscopy. Furthermore, flame retardancy and thermal property of various ethylene vinyl acetate copolymer (EVA) composites, including EVA/EG and EVA/EG/APP (ammonium polyphosphate) specimens, were studied through limiting oxygen index instrument (LOI), vertical combustion UL‐94 rating, thermal gravimetric and differential thermal analysis. The results indicate that the EVA/EG and EVA/EG/APP composites exhibit a better flame retardancy. Addition of EG at a mass fraction of 30% leads LOI of 70EVA/30EG composite improved to 28.7%. Even more, the synergistic effect between EG and APP improves the LOI of 70EVA/10APP /20EG composite to 30.7%. This synergistic efficiency is attributed to the formation of compact and stable layer‐structure, and the prepared EG can make EVA composite reach the UL‐94 level of V‐0. POLYM. COMPOS., 36:1407–1416, 2015. © 2014 Society of Plastics Engineers  相似文献   

5.
The halogen‐free flame retardant (HFFR) ethylene‐vinyl acetate copolymer (EVM)/ATH/SiO2 composites have been prepared by melting compounding method, and the flame retardant, thermal stability, rheological, electrical, and mechanical properties have been investigated by cone calorimeter, LOI, UL‐94, TG, FE‐SEM, rotational rheometer, dielectric breakdown, and ultimate tensile. The results indicate that the flame retardant of EVM vulcanizates is improved and the fire jeopardizing is dramatically reduced due to the addition of ATH. It is necessary that sufficient loading of ATH (≥120 phr) is needed to reach essential level (LOI > 30; V‐0 rating) of flame retardant for HFFR EVM/ATH/SiO2 composites used as cable in industry. The rheological characteristics show that at all the measurement frequencies, the storage and loss modulus of the composites increase monotonously as the concentration of ATH filler increases, while the complex viscosity and tan delta present reverse trend. And also, it has been found that the HFFR composites at high filler concentrations still keep good mechanical and electrical properties, which is very important for practical applications as cable. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010  相似文献   

6.
A novel flame retardant [9,10‐Dihydro‐9‐oxa‐10‐phosphaphenanthrene‐10‐oxideÔtriphosphazene (DOPO–TPN)] based on phosphaphenanthrene and cyclotriphosphazene was synthesized and used to improve the flame retardancy of poly(ethylene terephthalate) (PET). The structure of DOPO–TPN was characterized by nuclear magnetic resonance, Fourier transform infrared spectroscope (FTIR), and elemental analysis. PET/DOPO–TPN composites with different amount of DOPO–TPN were prepared and the flame retardancy was determined by limiting oxygen index (LOI) and vertical burning test (UL‐94). With the incorporation of 5 wt % DOPO–TPN, the composite achieved a LOI value of 34% and UL‐94 V‐0 rating. The thermal properties of the PET/DOPO–TPN composites were investigated by thermogravimetric analysis. The flame retardant mechanism was investigated by pyrolysis‐gas chromatography/mass spectrometry (Py‐GC/MS), FTIR, and scanning electron microscopy (SEM). The Py‐GC/MS results showed that DOPO based fragments would exist in the gas phase during the pyrolysis of PET/DOPO–TPN composites which demonstrated that DOPO–TPN could act through gas‐phase action to exert flame retardant effect. The results of FTIR and SEM demonstrated that DOPO–TPN could promote the formation of compact and intact char residues to inhibit the heat and combustible gas transmission in condensed phase. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45246.  相似文献   

7.
This work aims to develop halogen‐free poly(1,4‐butylene terephthalate) (PBT) composites with enhanced flame retardancy using ecofriendly flame retardants, aluminum hypophosphite (AHP) and melamine derivatives (melamine polyphosphate and melamine cyanurate). Microscale combustion calorimetry and thermal gravimetric analysis/infrared spectrometry (TG‐IR) technique were used to investigate the potential fire hazards of these PBT composites. For the PBT composites with the incorporation of AHP and melamine derivatives, the heat release capacity (HRC) which is an indicator of a material fire hazard was significantly reduced, and the intensities of a variety of combustible or toxic gases detected by TG‐IR technique were remarkably decreased. Moreover, a loading of 20 wt % flame retardant mixture fulfilled the PBT composites high limited oxygen index (LOI) and V‐0 classification in UL 94 testing. An intumescent flame retarded mechanism was speculated in this work, because numerous bubble‐like char residues were found on the surface of the samples containing flame retardant mixture after LOI testing. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011  相似文献   

8.
A novel silicone‐containing flame retardant (HSOBA) synthesized from hydrogen‐containing silicone oil and Bisphenol A via a simple approach has been incorporated into polycarbonate (PC) matrix to study its effects on the flame retardancy. The flame retardancy of PC/HSOBA composites is investigated by limiting oxygen index (LOI), vertical burning tests (UL‐94), and cone calorimeter measurement. The LOI value of the composites is 31.7 and the UL‐94 rating reaches V‐0, when the content of HSOBA is 3 wt %. Cone calorimeter data confirm that the HSOBA acts as an effective additive functioning both as flame retardants and as smoke suppressant. Evolution of the thermal behaviors of the composites tested by TGA, the morphological structures, and the constituent of char residue after LOI tests characterized by scanning electronic microscopy‐energy‐dispersive X‐ray analysis were used to explain the possible flame‐retardant mode. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012  相似文献   

9.
A novel intumescent flame retardant (IFR), containing ammonium polyphosphate (APP) and poly(tetramethylene terephthalamide) (PA4T), was prepared to flame‐retard acrylonitrile‐butadiene‐styrene (ABS). The flame retardation of the IFR/ABS composite was characterized by limiting oxygen index (LOI) and UL‐94 test. Thermogravimetric analysis (TGA) and TGA coupled with Fourier transform infrared spectroscopy (TG‐FTIR) were carried out to study the thermal degradation behavior of the composite and look for the mechanism of the flame‐retarded action. The morphology of the char obtained after combustion of the composite was studied by scanning electron microscopy (SEM). It has been found the intumescent flame retardant showed good flame retardancy, with the LOI value of the PA4T/APP/ABS (7.5/22.5/70) system increasing from 18.5 to 30% and passing UL‐94 V‐1 rating. Meanwhile, the TGA and TG‐FTIR work indicated that PA4T could be effective as a carbonization agent and there was some reaction between PA4T and APP, leading to some crosslinked and high temperature stable material formed, which probably effectively promoted the flame retardancy of ABS. Moreover, it was revealed that uniform and compact intumescent char layer was formed after combustion of the intumescent flame‐retarded ABS composite. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012  相似文献   

10.
Pentaerythritol phosphate melamine salt (PPMS) as a single‐molecule intumescent fire retardant was synthesized and characterized. The influence of the PPMS content on the combustion and thermal decomposition processes of intumescent‐flame‐retardant (IFR) ethylene–vinyl acetate copolymer (EVA) composites was studied by limiting oxygen index (LOI) measurement, UL 94 rating testing, cone calorimetry, thermogravimetric analysis, and scanning electron microscopy. The LOI and UL 94 rating results illustrate that PPMS used in EVA improved the flame retardancy of the EVA composites. The cone calorimetry test results show that the addition of PPMS significantly decreased the heat‐release rate, total heat release, and smoke‐production rate and enhanced the residual char fire performance of the EVA composites. The IFR–EVA3 composite showed the lowest heat‐release and smoke‐production rates and the highest char residue; this means that the IFR–EVA3 composite had the best flame retardancy. The thermogravimetry results show that the IFR–EVA composites had more residual char than pure EVA; the char residue yield increased with increasing PPMS content. The analysis results for the char residue structures also illustrated that the addition of PPMS into the EVA resin helped to enhance the fire properties of the char layer and improve the flame retardancy of the EVA composites. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42148.  相似文献   

11.
In this work, cerium hypophosphite (CeHP) was synthesized and characterized by scanning electron microscope (SEM) and thermogravimetric analysis (TGA) test. CeHP presented rod‐like morphological feature with good thermal stability. Subsequently, CeHP was added into glass fiber reinforced polyamide 6 (GFPA) to develop flame retardant glass fiber reinforced polyamide 6 composites (FR‐GFPA). The flame retardancy of FR‐GFPA composites was characterized by limiting oxygen index (LOI), Underwriters Laboratories 94 testing (UL‐94), microscale combustion calorimeter, and cone calorimeter test. FR‐GFPA composite with 20 wt% CeHP loading passed UL‐94 V0 rating with a high LOI of 26.5 vol%. Cone Calorimeter test showed that peak of heat release rate (PHRR) and total heat release (THR) of FR‐GFPA composites were reduced 27.1% and 21.1% compared with those of GFPA. The mechanical measurement revealed that the tensile strength first increased and then decreased with the increase of CeHP loading. With 15 wt% CeHP loading, the tensile strength of FR‐GFPA composite was 43.0% higher than GFPA. TGA and char residue characterization revealed that the addition of CeHP could significantly promote the formation of condensed char residue. The FR‐GFPA composites obtained herein exhibited superior combined properties of fire resistance, thermal stability, and mechanical properties, demonstrating that CeHP will be a promising candidate for preparing high performance polyamide composites. POLYM. COMPOS., 37:3073–3082, 2016. © 2015 Society of Plastics Engineers  相似文献   

12.
A novel flame retardant, tetra(5,5‐dimethyl‐1,3‐ dioxaphosphorinanyl‐2‐oxy) neopentane (DOPNP), was synthesized successfully, and its structure was characterized by FT‐IR, 1H NMR, and 31P NMR. The thermogravimetric analysis (TGA) results demonstrate that DOPNP showed a good char‐forming ability. Its initial decomposition temperature was 236.4°C based on 1% mass loss, and its char residue was 41.2 wt % at 600°C, and 22.9 wt % at 800°C, respectively. The flame retardancy and thermal degradation behavior of novel intumescent flame‐retardant polypropylene (IFR‐PP) composites containing DOPNP were investigated using limiting oxygen index (LOI), UL‐94 test, TGA, cone calorimeter (CONE) test, and scanning electron microscopy (SEM). The results demonstrate that DOPNP effectively raised LOI value of IFR‐PP. When the loading of IFR was 30 wt %, LOI of IFR‐PP reached 31.3%, and it passed UL‐94 V‐0. TGA results show that DOPNP made the thermal decomposition of IFR‐PP take place in advance; reduced the thermal decomposition rate and raised the residual char amount. CONE results show that DOPNP could effectively decrease the heat release rate peak of IFR‐PP. A continuous and compact char layer observed from the SEM further proved the flame retardance. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011.  相似文献   

13.
In this work, the flammability behaviors and synergistic effects of red phosphorus masterbatch (RPM) with expandable graphite (EG) in flame‐retardant high‐density polyethylene/ethylene vinyl‐acetate copolymer (HDPE/EVA) composites have been investigated by limiting oxygen index (LOI), UL‐94 test, cone calorimeter test (CCT), thermogravimetric analysis (TGA), Fourier‐transform infrared (FTIR) and scanning electron microscopy (SEM). The data obtained from LOI, UL‐94 test and CCT showed that suitable amount of RPM had synergistic effects with EG in the HDPE/EVA/EG/RPM composites. The addition of RPM greatly increased the LOI values by 3.4%, obtained UL‐94 V‐0 rating, decreased the heat release rates and total heat release, and prolongated the ignition time when 6.7 phr RPM substituted for EG in the HDPE/EVA/EG/RPM composites. The data from TGA and FTIR spectra also indicated the synergistic effects of RPM with EG considerably enhanced the thermal degradation temperatures. The morphological observations after UL‐94, CCT, and SEM images presented positive evidences that the synergistic effects took place for RPM with EG, and the flame‐retardant mechanism has been changed in flame‐retardant HDPE/EVA/EG/RPM composites. The formation of stable and compact charred residues promoted by RPM acted as effective heat barriers and thermal insulations, which improved the flame‐retardant performances and prevented the underlying polymer materials from burning. POLYM. ENG. SCI., 55:2884–2892, 2015. © 2015 Society of Plastics Engineers  相似文献   

14.
Aluminum hypophosphite (AHP), a novel flame retardant, was used to improve the flame retardancy of low‐density polyethylene (LDPE) with microencapsulated red phosphorus (MRP). The synergistic effect between MRP and AHP was investigated by the limiting oxygen index (LOI), vertical burning test (UL‐94), and thermogravimetric analysis. When the contents of MRP and AHP were 10 and 30 phr, the LOI of LDPE/10MRP/30AHP composite was 25.5%, and it passed the UL‐94 V‐0 rating (the number before “MRP” and “AHP” is the loading of MRP and AHP, In LDPE/10MRP/30AHP, the content of the LDPE, MRP and AHP is 100phr, 10phr and 30phr, where phr refers to parts per hundreds of resin). The results of cone calorimetry testing show that the heat release rate of the composites was significantly reduced, and the strength of the char layer improved when the loading of AHP increased. The thermal stability of the LDPE/10MRP/30AHP composite was enhanced. The structure of the char was investigated by Fourier transform infrared spectrometry and scanning electron microscopy/energy‐dispersive spectrometry. The results indicate that AHP promoted the formation of stable char. This research provided a good way to prepare flame‐retardant materials with a halogen‐free flame retardant and contributed to environmental protection. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43225.  相似文献   

15.
A novel phosphorous-nitrogen structure containing intumescent flame retardant, 4,4-diaminodiphenyl methane bi(2,2-dimethyl-1,3-propanediol) phosphoramidate (DBDPP) was synthesized and characterized. Thermal stability and flammability properties of ethylene vinyl-acetate copolymer rubber(EVM)/DBDPP composites were investigated by thermogravimetric analysis (TGA), limiting oxygen index (LOI) test and UL-94 measurement, respectively. The results showed that the addition of DBDPP enhanced the thermal stability and flame retardancy of EVM significantly. The weight of residues improved greatly with the addition of DBDPP. SEM investigations revealed that a strong charred layer was formed from EVM/DBDPP composites during combustion. It is confirmed that the char structure was a critical factor for flame retardancy of EVM rubber. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012  相似文献   

16.
Microencapsulated ammonium polyphosphate (MUFAPP) with a double shell is prepared by in situ polymerization, and is characterized by FTIR, XPS and SEM, etc. The microencapsulation of APP can increase its flame retardance and water resistance in PP. The flame retardant action of MUFAPP and APP in PP are studied using LOI and UL 94 test, and their thermal stability is evaluated by TG. The LOI value of the PP/MUFAPP composite at the same loading is higher than that of PP/APP composite. The LOI values of the PP/MUFAPP/ dipentaerythritol are higher than that of the PP/MUFAPP, and UL 94 ratings of most ternary composites are raised to V-0 at 30 wt.% loading. The results of the cone calorimeter also indicate that MUFAPP is an effective flame retardant in PP. The thermal degradation behaviors of APP and MUFAPP are studied using TG and dynamic FTIR.  相似文献   

17.
Vinyl polysiloxane microencapsulated ammonium polyphosphate (MAPP) was prepared by a sol-gel method using vinyltrimethoxysilane as a precursor to improve its thermal stability and hydrophobicity. The MAPP was characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy dispersive spectrometer (EDS) and thermogravimetric analyzer (TGA). The results showed that ammonium polyphosphate (APP) was successfully coated with vinyl polysiloxane. MAPP and pentaerythritol (PER) were used together to improve the flame retardancy of polypropylene (PP). The flame retardant properties of PP composites were investigated by limiting oxygen index (LOI), UL-94 test, TGA and SEM. When the MAPP was added as a flame retardant, with PER as a char forming agent, the LOI of PP/MAPP/PER composites was 33.1%, and it reached the UL-94 V-0 level. The results also demonstrated that the flame retardant properties of PP/MAPP/PER composites were better than those of PP/APP/PER composites at the same loading. Moreover, the addition of flame retardant and carbon forming agent could promote the crystallization behavior of PP.  相似文献   

18.
Tris(2‐hydroxyethyl) isocyanurate (THEIC) was used as charring agent and combined with ammonium polyphosphate (APP) to form an intumescent flame retardant (IFR) for polypropylene (PP). The flame retardancy and combustion performance of PP/IFR composite was tested by limiting oxygen index (LOI), UL‐94 vertical burning test and cone calorimeter. The results showed that PP/IFR composite had highest LOI of 34.8 and obtained V‐0 rating when 30 wt % IFR was loaded and mass ratio APP/THEIC was 2 : 1. The peak heat release (PHRR) and total heat release (THR) values of PP composite containing FRs were remarkably reduced compared with that of pure PP. However, water resistant test demonstrated the PP/IFR composite had poor flame retardant durability, both the LOI value and UL‐94 V‐rating decreased when PP/IFR composite was soaked in water at 70°C after 36 h. The degradation process and the char morphology of IFR and PP/IFR composite were investigated by TGA and SEM images. The possible reaction path between APP and THEIC in the swollen process was proposed. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41214.  相似文献   

19.
The flammability of polypropylene (PP) composites containing intumescent flame‐retardant additives, i.e., melamine pyrophosphate (MPP) and 1‐oxo‐4‐hydroxymethyl‐2,6,7‐trioxa‐1‐phosphabicyclo[2.2.2]octane (PEPA) was characterized by limiting oxygen index (LOI), UL 94 test, and cone calorimeter. In addition, the thermal degradation of the composites was studied using thermogravimetric analysis (TG) and real‐time Fourier transform infrared (RTFTIR). It has been found that the PP composite only containing MPP (or PEPA) does not show good flame retardancy even at 30% additive level. Compared with the PP/MPP binary composite, the LOI values of the PP/MPP/PEPA ternary composites at the same additive loading are all increased, and UL 94 rating of the ternary composite (PP3) studied is raised to V‐0 rating from no rating (PP/MPP). The cone calorimeter results show that the heat release rate of some ternary composites decreases in comparison with the binary composite. It is noted from the TG data that initial decomposition temperatures of ternary composites are lower than that of the binary composites. The RTFTIR study indicates that the PP/MPP/PEPA composites have higher thermal oxidative stability than the pure PP. POLYM. ENG. SCI., 2010. © 2009 Society of Plastics Engineers  相似文献   

20.
A novel flame retardant (SPDH) containing phosphorus was synthesized through the reaction of 10‐(2, 5‐dihydroxyphenyl)‐9, 10‐dihydro‐9‐oxa‐10‐phosphaphenanthrene‐10‐oxide (DOPO‐HQ) and synthesized intermediate product 3, 9‐dichloro‐2, 4, 8, 10‐tetraoxa‐3, 9‐diphosphaspiro(5.5)undecane‐3, 9‐dioxide (SPDPC). The structure and properties of SPDPC and SPDH were characterized by Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance (NMR) spectroscopy and thermogravimetric analysis (TGA). After blending with poly(ethylene‐co‐vinyl acetate) (EVA), the flame‐retardant properties of EVA/SPDH composites were estimated by cone calorimeter, limited oxygen index (LOI) and UL‐94 tests, whereas the thermal stabilities were investigated using TGA. The morphological microstructure of the char formed by EVA/SPDH composite after combustion in cone calorimeter was investigated by scanning electron microscopy (SEM). The results indicate that the flame retardant and thermal stability were improved by incorporation of SPDH. The rich foamy char layers were observed from the residues after combustion in a cone calorimeter, which exactly benefits the improvement of thermal stability and flame retardant property of materials. Copyright © 2010 John Wiley & Sons, Ltd.  相似文献   

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