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1.
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   

2.
李斌 《高分子科学》2015,33(2):318-328
The effects of aluminum hypophosphite(AHP) as a synergistic agent on the flame retardancy and thermal degradation behavior of intumescent flame retardant polypropylene composites(PP/IFR) containing ammonium polyphosphate(APP) and triazine charring-foaming agent(CFA) were investigated by limiting oxygen index(LOI), UL-94 measurement, thermogravimetric analysis(TGA), cone calorimeter test(CONE), scanning electron microscopy(SEM) and X-ray photoelectron spectroscopy(XPS). It was found that the combination of IFR with AHP exhibited an evident synergistic effect and enhanced the flame retardant efficiency for PP matrix. The specimens with the thickness of 0.8 mm can pass UL-94 V-0 rating and the LOI value reaches 33.5% based on the total loading of flame retardant of 24 wt%, and the optimum mass fraction of AHP/IFR is 1:6. The TGA data revealed that AHP could change the degradation behavior of IFR and PP/IFR system, enhance the thermal stability of the IFR and PP/IFR systems at high temperatures and promote the char residue formation. The CONE results revealed that IFR/AHP blends can efficiently reduce the combustion parameters of PP, such as heat release rate(HRR), total heat release(THR), smoke production rate(SPR) and so on. The morphological structures of char residue demonstrated that AHP is of benefit to the formation of a more compact and homogeneous char layer on the materials surface during burning. The analysis of XPS indicates that AHP may promote the formation of sufficient char on the materials surface and improve the flame retardant properties.  相似文献   

3.
Ferric pyrophosphate (FePP) was added to an ammonium polyphosphate (APP)—pentaerythritol (petol) intumescent flame retardant (IFR) system in polypropylene (PP) matrix, with subsequent investigation into the synergistic effect between FePP and the IFRs. Limited oxygen index (LOI), UL‐94 test and cone calorimeter test were employed to study the flame retardance of the synthesized flame retardant PP composites. Thermogravimetric analysis (TGA) and thermogravimetric analysis‐infrared spectrometry (TG‐IR) were used to study their thermal degradation characteristics and gas products. TG‐IR results demonstrate that there is no Fe (CO)5 produced from PP/IFR/FePP system, which implies that the flame retardant mechanism of PP/IFR/FePP system is in the condensed phase rather than in the gas phase. Real time FTIR and X‐ray photoelectron spectroscopy (XPS) were used to monitor the thermal oxidative stability and the high temperature performance of the flame retardant PP composites. The real time FTIR spectra show that all peaks around 2900 cm?1 almost disappear at 380°C for the PP/IFR system, meaning that PP decomposes completely at this temperature. But after the addition of 2 wt%wt% FePP, the peaks still exist till 400°C. XPS shows that the aliphatic carbon atom content in PP/23 wt%wt% IFR/2 wt%wt% FePP (63.8%) is much higher than the one without FePP, and the total oxygen atom content in PP/23 wt%wt% IFR/2 wt%wt% FePP is just 19.1%, while the one in PP/25 wt% IFR is as high as 35.7%. Copyright © 2009 John Wiley & Sons, Ltd.  相似文献   

4.
Polypropylene/intumescent flame retardant/organophilic Fe-montmorillonite (PP/IFR/Fe-OMT) nanocomposites were prepared by melting intercalation. In order to investigate the effect of structural Fe3+ in the PP/IFR system, the corresponding PP/IFR and PP/IFR/Na-OMT composites were prepared under the same conditions. The thermo-gravimetric analysis data show that the PP/IFR/Fe-OMT nanocomposites have higher thermal stability than the PP/IFR and PP/IFR/Na-OMT composites. The flame retardant results indicate that the limiting oxygen index values of the nanocomposites with Fe-OMT are basically higher than those of the pure PP and the composites containing IFR or Na-OMT/IFR. And the addition of a suitable amount of Fe-OMT in PP/IFR composites can apparently favor UL94 test, and no dripping phenomenon was found. The cone calorimeter test indicates that the heat release rate (HRR) is significantly reduced by the formation of the nanocomposites, and the HRR of the PP/IFR/Fe-OMT nanocomposites are decreased in comparison with those of the PP/IFR/Na-OMT nanocomposites. It is noteworthy that Fe-OMT is helpful to smoke suppression by smoke density test.  相似文献   

5.
A novel ionic liquid containing phosphorus ([PCMIM]Cl) was synthesized and characterized by FTIR, 1H NMR, 13C NMR and 31P NMR. Moreover, a new intumescent flame retardant (IFR) system, which was composed of [PCMIM]Cl and ammonium polyphosphate (APP), was used to impart flame retardancy and dripping resistance to polypropylene (PP). The flammability and thermal behaviors of intumescent flame‐retarded PP (PP/IFR) composites were evaluated by limiting oxygen index (LOI), UL‐94 test, thermogravimetric analysis (TGA) and cone calorimeter test. It was found that there was an obvious synergistic effect between [PCMIM]Cl and APP. When the weight ratio of [PCMIM]Cl and APP was 1:5 and the total amount of IFR was kept at 30 wt%, LOI value of PP/IFR composite reached 31.8, and V‐0 rating was obtained. Moreover, both the peak heat release rate and the peak mass loss rate of PP/IFR composites decreased significantly relative to PP and PP/APP composite from cone calorimeter analysis. The TGA curves suggested that [PCMIM]Cl had good ability of char formation, and when combined with APP, it could greatly promote the char formation of PP/IFR composites, hence improved the flame retardancy. Additionally, the rheological behaviors and mechanical properties of PP/IFR composites were also investigated, and it was found that [PCMIM]Cl could also serve as an efficient lubricant and compatibilizer between APP and PP, endowing the materials with satisfying processability and mechanical properties. Copyright © 2013 John Wiley & Sons, Ltd.  相似文献   

6.
Piperazine cyanurate (PCA) is designed and synthesized via hydrogen‐bonding self‐assembly reactions between piperazine and cyanuric acid. Chemical structure and morphology of PCA are investigated by Fourier transform infrared spectroscopy and scanning electron microscopy, respectively. The prepared PCA is combined with ammonium polyphosphate (APP) to prepare flame‐retardant polypropylene (PP) composites. Thermostability, flammability, and combustion characteristics of PP composites are analyzed. The maximum thermal decomposition rate of flame‐retarded PP composites has an apparent reduction compared with that of pure PP, and obvious char is left for this intumescent flame retardant (IFR) system of APP and PCA. A high limiting oxygen index value and UL‐94 V‐0 rating are achieved with addition of APP and PCA. In cone calorimetry test, heat and smoke releases of PP are significantly decreased by this IFR system. Gaseous decomposition products during the thermal decomposition of flame‐retardant composites are studied. Chemical structure and morphology of char residues are analyzed. The results illustrate that APP and PCA have a superb synergistic action in the aspect of improvement in fire safety of PP. A possible flame‐retardant mechanism is concluded to reveal the synergism between APP and PCA.  相似文献   

7.
The synergistic effects of 4A zeolite (4A) on the thermal degradation, flame retardancy and char formation of a novel halogen‐free intumescent flame retardant polypropylene composites (PP/IFR) were investigated by the means of limiting oxygen index (LOI), vertical burning test (UL‐94), digital photos, scanning electron microscopy (SEM), thermogravimetric analysis (TGA), cone calorimeter test (CCT), laser Raman spectroscopy (LRS) and X‐ray photoelectron spectroscopy (XPS). It was found that a small amount of 4A could dramatically enhance the LOI value of the PP/IFR systems and the materials could pass the UL‐94 V‐0 rating test. Also, it could enhance the fire retardant performance with a great reduction in combustion parameters of PP/IFR system from CCT test. The morphological structures observed by digital and SEM photos revealed that 4A could promote PP/IFR to form more continuous and compact intumescent char layer. The LRS measurement, XPS and TGA analysis demonstrated that the compactness and strength of the outer char surface of the PP/IFR/4A system was enhanced, and more graphite structure was formed to remain more char residue and increase the crosslinking degree. Copyright © 2013 John Wiley & Sons, Ltd.  相似文献   

8.
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   

9.
In this paper, three typical transition metal phosphide nanocrystallines (MxPy, M = Ni, Co, and Cu) were synthesized by a novel hydrothermal method, and their structures were characterized by X‐ray diffraction and transmission electron microscopy. Then they were used as synergistic agents with intumescent flame retardant (IFR) to improve the fire safety of polypropylene (PP). Thermogravimetry analysis (TGA) results indicated that the introduction of these synergists could improve the thermal stability and char yields of the PP/IFR system. The addition of 2 wt.% Ni12P5 and Co2P increased the limiting oxygen index values of the PP/IFR system significantly from 28% to 36% and 34%, respectively, and the system could reach V‐0 rating. The cone calorimeter test results revealed that the combination of transition metal phosphide nanocrystallines and IFR system could result in excellent flame retardancy. The incorporation of these synergists into IFR led to a remarkable influence on charring of PP composites as revealed by TGA and cone data. The morphological structure of char residue proved that the addition of transition metal phosphide nanocrystallines was capable of forming a compact and homogeneous char on the surface, which turned out to be of most importance for the flame retardancy. Thermogravimetric analysis/infrared spectrometry results indicated that the flame retardant mechanism of PP/IFR/MxPy (M = Ni, Co, and Cu) system was in the condensed phase rather than in the gas phase. Copyright © 2014 John Wiley & Sons, Ltd.  相似文献   

10.
Three kinds of organic intercalation agent containing flame retardant groups, melamine (MA), triphenylphonium (TPP) chloride, and tetradecyl trihexyl phosphonium (TTP) bromide were intercalated into montmorillonite (MMT) via cation exchange reactions. These modified MMTs are combined with intumescent systems and compounded with PP. The flame retardant and thermal properties of the PP composites are studied. The organic intercalation agents in the layers of MMT play important roles in the char formation and flame retardant properties of PP composites. MA shows a better performance in limiting oxygen index (LOI) value and TPP helps to increase UL‐94 properties, whereas TTP maintains or deteriorates the flame retardancy of polypropylene/intumescent flame retardant (IFR) composites. The LOI and UL‐94 properties increase firstly and then decrease as the content of MMT increases. The MA acts as a blowing agent and emits an inert gas to provide migration impetus, which results in a better intumescent structured and stronger char to endure heat erosion. Although TPP and TTP emit combustible gas that burn, especially for TTP as it has a more flammable aliphatic chain. The synergistic effect between MA‐MMT and IFR is better than that for TPP‐MMT and TTP‐MMT. Copyright © 2014 John Wiley & Sons, Ltd.  相似文献   

11.
Organically modified montmorillonite (OMMT) was used as synergist to enhance the flame-retardant and mechanical properties of poly(butylene succinate)/intumescent flame retardant (PBS/IFR) composites. The flame-retardant, thermal degradation and combustion properties of PBS and its flame-retardant composites were characterized by limiting oxygen index (LOI) test, vertical burning (UL-94) test, thermogravimetric analysis, cone calorimeter and scanning electron microscopy, respectively. The results indicate that PBS/IFR composites exhibit excellent flame retardance when OMMT is at an appropriate content. PBS/IFR composite with 20 wt% IFR and 1.5 wt% OMMT has an LOI of 40.1% and can pass the UL-94 V0 rating. The synergistic effect between OMMT and IFR on the flame-retardant properties of PBS depends on the content of OMMT, and excessive OMMT diminish this synergistic effect. The possible flame-retardant mechanism of OMMT on PBS/IFR composite is proposed. The results of mechanical test also indicate that OMMT can effectively increase the notched impact strength of PBS/IFR composites.  相似文献   

12.
The flame retardancy of a novel intumescent flame‐retardant polypropylene (IFR‐PP) system, which was composed of a charring agent (CA), ammonium polyphosphate (APP), and polypropylene (PP), could be enhanced significantly by adding a small amount (1.0 wt%) of an organic montmorillonite (O‐MMT). The synergistic flame‐retardant effect was studied systematically. The thermal stability and combustion behavior of the flame‐retarded PP were also investigated by thermogravimetric analysis (TGA), limiting oxygen index (LOI), vertical burning test (UL‐94), scanning electronic microscopy (SEM), and cone calorimeter test (CCT). TGA results demonstrated that the onset decomposition temperatures of IFR‐PP samples, with or without O‐MMT, were higher than that of neat PP. Compared with IFR‐PP, the LOI value of IFR‐PP containing 1.0 wt% O‐MMT was increased from 30.8 to 33.0, and the UL‐94 rating was also enhanced to V‐0 from V‐1 when the total loading of flame retardant was the same. The cone calorimeter results showed that the IFR‐PP with 1.0 wt% of O‐MMT had the lowest heat release rate (HRR), total heat release (THR), total smoke production (TSP), CO production (COP), CO2 production (CO2P), and mass loss (ML) of all the studied IFR‐PP samples, with or without O‐MMT. All these results indicated that O‐MMT had a significantly synergistic effect on the flame‐retardancy of IFR‐PP at a low content of O‐MMT. Copyright © 2009 John Wiley & Sons, Ltd.  相似文献   

13.
The performances of the novel intumescent flame retardant (IFR) polypropylene (PP) composites containing melamine phosphate (MP) and tris(1‐oxo‐2,6,7‐trioxa‐1‐phosphabicyclo[2,2,2]methylene‐4)phosphate (TPMP) were investigated. The flame retardancy of IFR‐PP system was characterized by limiting oxygen index (LOI) and UL 94 and cone calorimeter. The morphology of the char obtained after cone calorimeter testing was studied by scanning electron microscopy (SEM). The thermal oxidative degradation (TOD) of the composites was investigated by using thermogravimetric analysis (TGA) and real‐time Fourier transform infrared spectroscopy (RT‐FTIR). Compared with the PP/ TPMP or PP/ MP binary composite, at the same addition level, the LOI values of the PP/MP/TPMP ternary composites increase and reach V‐0 at the suitable MP/TPMP ratio. The results of TGA and RT‐FTIR showed the existence of the interaction between IFR and PP. Copyright © 2008 John Wiley & Sons, Ltd.  相似文献   

14.
A novel intumescent flame retardant, containing ammonium polyphosphate (APP), and poly(hexamethylene terephthalamide) (PA6T), was prepared for flame retarding polypropylene (PP). The flame retardation of the PP composites was characterized by limiting oxygen index (LOI). The thermal degradation of the composites was investigated by means of thermogravimetric analysis (TG) and TG coupled with Fourier transform infrared spectroscopy (TG-FTIR). The morphology of the char obtained after combustion of the composites was studied by scanning electron microscopy. It has been found the intumescent flame retardant showed good flame retardancy, with the LOI value of the PA6T/APP/PP (5/25/70) system increasing from 17.5 to 32. Meanwhile, the TG and TG-FTIR work indicated that PA6T could be effective as a carbonization agent and there was a synergistic reaction between PA6T and APP, which effectively promoted the char formation of the PP composites. Moreover, it was revealed that uniform and compact intumescent char layer was formed after combustion of the intumescent flame retarded PP composites.  相似文献   

15.
The flammability of polypropylene (PP) composites containing intumescent flame retardant additives, i.e. melamine phosphate (MP) and pentaerythritol (PER), dipentaerythritol (DPER) or tripentaerythritol (TPER) was characterized by limiting oxygen index (LOI), UL 94 and the cone calorimeter, and 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 containing only MP does not show good flame retardancy even at 40% additive level. Compared with the PP/MP binary composite, the LOI values of the PP/MP/PER (PP/MP/DPER or PP/MP/TPER) ternary composites at the same additive loading are all increased, and UL 94 ratings of most ternary composites studied are raised to V-0 from no rating (PP/MP). The cone calorimeter results show that the heat release rate and smoke emission of some ternary composites decrease 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 composite. The RTFTIR study indicates that the PP/IFR composites have higher thermal oxidative stability than the pure PP.  相似文献   

16.
A new flame retardant system with organic modified boron nitride (m‐BN) and intumescent flame retardant (IFR) was used in this paper, and the synergistic flame retardancy of m‐BN and IFR on natural rubber (NR) was studied. NR/IFR/m‐BN composites were characterized by X‐ray photoelectron spectroscopy(XPS), Fourier transform infrared spectrometry (FTIR), thermogravimetric analysis, UL‐94, limiting oxygen index (LOI), tensile testing, cone calorimeter testing, and thermal conductivity testing. When 4 wt% m‐BN was added, the flame retardancy and mechanical properties of the composites were improved. The LOI value of NR/IFR/4 phr m‐BN reached 26.8%, and suppressed fire spread in a UL‐94 test. Compared with pure NR, the peak heat release rate (pHRR) was reduced by 52.2%, the total heat release (THR) was reduced by 27.6%, and CO yields were reduced by 51.4%. As a key aspect of fire safety, the ignition time is effectively delayed to 23 seconds due to the increased thermal conductivity of NR/IFR/m‐BN. Since the synergistic effect of m‐BN effectively improves the flame retardancy of NR, it provides a feasible method for improving the fire safety of polymers.  相似文献   

17.
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   

18.
Nanoflaky manganese phosphate (NMP) was synthesized from manganese nitrate and trisodium phosphate dodecahydrate, and used as a synergistic agent on the flame retardancy of polypropylene (PP)/intumescent flame retardant (IFR) system. The thermogravimetric analysis (TGA), real time Fourier-transform infrared (RTFTIR) spectroscopy measurements, cone calorimeter (CONE) and microscale combustion calorimeter (MCC) were used to evaluate the synergistic effects of NMP on PP/IFR system. When IFR + NMP was fixed at 20 wt% in flame retardant PP system, the TGA tests showed that NMP could enhance the thermal stability of PP/IFR system at initial temperature from about room temperature to 440 °C and effectively increase the char residue formation. The RTFTIR results revealed that NMP could clearly change the decomposition behavior of PP in PP/IFR system, which promotes decomposition at the initial temperature from about room temperature to 260 °C and forms more effective barrier layer to protect PP from decomposing at high temperature from about 260 °C to 500 °C. The CONE tests indicated that the addition of NMP in PP/IFR system not only reduced the peak heat release rate (HRR), but also prolonged the ignition time. The MCC results revealed that PP/IFR/NMP system generated less combustion heat over the course of heating than that of PP/IFR system. And scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) were used to explore the char residues of the PP/IFR systems with and without NMP.  相似文献   

19.
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   

20.
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   

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