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1.
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   

2.
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   

3.
Novel intumescent flame-retardant poly(lactic acid) (PLA/IFR)/organo-modified α-zirconium phosphate(OZrP) nanocomposites were prepared via incorporation of charring agent (CA), ammonium polyphosphate (APP) and OZrP into PLA. OZrP was synthesized directly by a solvent thermal method. The morphological characterization of PLA/IFR/OZrP nanocomposites was conducted by wide angle X-ray diffraction (WXRD) and transmission electron microscopy (TEM). The effect of the OZrP on flame retardancy and the thermal stability of PLA/IFR composites were studied by thermogravimetric analysis (TGA), limiting oxygen index (LOI), vertical burning test (UL-94) and cone calorimeter test. The TGA data illustrated that the OZrP could increase the residue and significantly improve the flame retardancy of PLA/IFR/OZrP nanocomposites showing an excellent synergistic effect. The addition of OZrP to the flame-retardant PLA increases the LOI and enhances the UL-94 rating. Cone calorimeter tests gave clear evidence that the incorporation of OZrP into PLA/IFR composites resulted in the significant reduction of the heat release rate (HRR), low total heat release (THR) and high amount of char residues during combustion. The flame-retardant mechanism of PLA/IFR/OZrP nanocomposites may correspond to the intumescent flame-retardant mechanism and catalyzed carbonization mechanism caused by OZrP.  相似文献   

4.
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   

5.
In order to modify the brittleness and flame retardant properties of poly(lactic acid) (PLA), a series of flame retardant toughened PLA composites were prepared using poly(ethylene glycol) 6000 (PEG6000) as a toughening and charring agent together with ammonium polyphosphate (APP) as an acid source and blowing agent. The fire and thermal behavior of PLA/PEG/APP composites was evaluated by limiting oxygen index (LOI), UL‐94, cone calorimeter, and thermogravimetric analysis (TGA). The results showed that the PLA/PEG/APP system had good charring ability and could improve the flame retardancy of PLA. When the content of APP in the composites was more than 5 wt%, all samples could reach UL‐94 V‐0 rating. The results of mechanical property tests demonstrated that the brittleness of PLA was also improved after blended with PEG6000. All the PLA/PEG/APP composites with an APP content of less than 10 wt% showed an obvious neck and fracture behavior, that is, the tensile behavior of PLA was changed from brittle to ductile. Copyright © 2010 John Wiley & Sons, Ltd.  相似文献   

6.
The flame retardancy mechanisms of poly(1,4‐butylene terephthalate) (PBT) containing microencapsulated ammonium polyphosphate (MAPP) and melamine cyanurate (MC) were investigated via pyrolysis analysis (thermogravimetric analysis (TGA), real‐time Fourier transform infrared (FTIR), TG‐IR), cone calorimeter test, combustion tests (limited oxygen index (LOI), UL‐94), and residue analysis (scanning electron microscopy (SEM)). A loading of 20 wt% MC to PBT gave the PBT composites an LOI of 26%, V‐2 classification in UL‐94 test and a high peak heat release rate (HRR) in cone calorimeter test. Adding APP to PBT/MC composites did not improve their flame retardancy. In comparison with the addition of ammonium polyphosphate (APP) to PBT, MAPP with silica gel shell and MAPP with polyurethane shell both promoted the intumescent char‐forming and improved the flame retardancy of PBT through different mechanisms in the presence of MC. These two halogen‐free PBT composites with V‐0 classification according to UL‐94 test were obtained; their LOI were 32 and 33%, respectively. Copyright © 2010 John Wiley & Sons, Ltd.  相似文献   

7.
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   

8.
A systematic series of flexible polyurethane foams (FPUF) with different concentrations of flame retardants, bis([dimethoxyphosphoryl]methyl) phenyl phosphate (BDMPP), and melamine (MA) or expandable graphite (EG) was prepared. The mechanical properties of the FPUFs were evaluated by a universal testing machine. The pyrolysis behaviors and the evolved gas analysis were done by thermogravimetric analysis (TGA) and TGA coupled with Fourier-transform infrared (TG-FTIR), respectively. The fire behaviors were studied by limiting oxygen index (LOI), UL 94 test for horizontal burning of cellular materials (UL 94 HBF), and cone calorimeter measurement. Scanning electronic microscopy (SEM) was used to examine the cellular structure's morphology and the postfire char residue of the FPUFs. LOI and UL 94 HBF tests of all the flame retarded samples show improved flame retardancy. BDMPP plays an essential role in the gas phase because it significantly reduces the effective heat of combustion (EHC). This study highlights the synergistic effect caused by the combination of BDMPP and EG. The measured char yield from TGA is greater than the sum of individual effects. No dripping phenomenon occurs during burning for FPUF-BDMPP-EGs, as demonstrated by the result of the UL 94 HBF test. EG performs excellently on smoke suppression during burning, as evident in the result of the cone calorimeter test. MA reduces the peak heat release rate (pHRR) significantly. The synergistic effect of the combination of BDMPP and EG as well as MA offers an approach to enhance flame retardancy and smoke suppression.  相似文献   

9.
利用9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)和马来酸酐(MA)对淀粉进行改性得到磷化淀粉(DOPOMASt),通过红外光谱(FTIR)、核磁共振谱(1H-NMR)和X射线光电子能谱(XPS)确定其结构.利用DOPOMASt作为碳源,与聚磷酸铵(APP)复配后通过熔融共混制备了阻燃聚乳酸(PLA)...  相似文献   

10.
A hyperbranched polyamine was prepared using an A2 + B3 approach. It acted as a hyperbranched charring and foaming agent (HCFA) in combination with ammonium polyphosphate (APP) to form a new intumescent flame retardant (IFR) system for polyamide 6 (PA6). Effect of HCFA on flame retardant and thermal degradation properties of IFR‐PA6 was investigated by limiting oxygen index (LOI), UL‐94 vertical burning, cone calorimeter, and thermogravimetric analysis (TGA) tests. The IFR system presented the most effective flame retardancy in PA6 when the weight ratio of APP to HCFA was 2:1. The LOI value of IFR‐PA6 could reach 36.5 with V‐0 rating when the IFR loading was 30 wt%. Even if the loading decreased to 25 wt%, IFR‐PA6 could still maintain V‐0 rating with an LOI value of 31. TGA curves indicated that APP would interact with both PA6 and HCFA in PA6/APP/HCFA composite under heating. The interaction between APP and HCFA improved the char formation ability of IFR system and then much more char was formed for PA6/APP/HCFA composite than for PA6/APP. Therefore, better flame retardancy was achieved. Moreover, the structure and morphology of char residue were studied by Fourier transform infrared (FTIR), X‐ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM). The results indicated that compact and foaming char layer containing P‐O‐C structure was formed for PA6/APP/HCFA system during combustion. Copyright © 2010 John Wiley & Sons, Ltd.  相似文献   

11.
In this work, the flame‐retardant high‐density polyethylene/ethylene vinyl‐acetate copolymer (HDPE/EVA) composites have been prepared by using expandable graphite (EG) as a flame retardant combined with ammonium polyphosphate (APP) and red phosphorus masterbatch (RPM) as synergists. The synergistic effects of these additives on the flammability behaviors of the filled composites have been investigated by limiting oxygen index, UL‐94 test, cone calorimeter test, thermogravimetric analysis (TGA), Fourier‐transform infrared (FTIR), and scanning electron microscopy. The results show that APP and RPM are good synergists for improving the flame retardancy of EG‐filled HDPE/EVA composites. The data from TGA and FTIR spectra also indicate the synergistic effects of APP and RPM with EG considerably enhance the thermal degradation temperatures but decrease the charred residues of the HDPE/EVA/EG composites because the flame‐retardant mechanism has changed. The morphological observations present positive evidences that the synergistic effects take place in APP and RPM with EG in flame‐retardant EG‐filled HDPE/EVA/EG composites. The formation of stable and compact charred residues promoted by APP and RPM with EG acts as effective heat barriers and thermal insulations, which improves the flame‐retardant performances and prevents the underlying polymer materials from burning. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

12.
A novel functionalized α-zirconium phosphate (F-ZrP) modified with intumescent flame retardant was synthesized by co-precipitation method and characterized. Poly (lactic acid) (PLA)/F-ZrP nanocomposites were prepared by melt blending method. The thermal stability and combustion behavior of PLA/F-ZrP nanocomposites were investigated by thermogravimetric analysis (TGA), limiting oxygen index (LOI), vertical burning test (UL-94), scanning electronic microscopy (SEM), and cone calorimeter test (CCT). The results showed that the addition of flame retardant F-ZrP slightly affect PLA's thermal stability, but significantly improve the flame retardancy of PLA composites. In comparison with neat PLA, the LOI value of PLA/F-ZrP was increased from 19.0 to 26.5, and the UL-94 rating was enhanced to V-0 as the loading of F-ZrP at 10%. SEM results suggested the introduction of F-ZrP in the PLA system can form compact intumescent char layer during burning. All these results showed that the F-ZrP performed good flame retardancy for PLA.  相似文献   

13.
采用热失重、X-射线光电子能谱分析、氧指数及烟密度测试等方法研究了可膨胀石墨(EG)与聚磷酸铵(APP)复配膨胀阻燃硬质聚氨酯泡沫塑料(RPUF)的热降解、燃烧性能及产烟行为.在此基础上利用锥形量热仪考察了EG/APP对磷酸三(β-氯异丙基)酯(TCPP)阻燃RPUF体系燃烧性能的影响.研究表明,EG与APP间的相互作用导致了EG/APP体系高温阶段失重速率下降、残炭量显著上升;EG/APP与RPUF之间的成炭作用以APP的化学成炭为主.与RPUF比较,RPUF/EG/APP的氧指数由19.8%提高至35.4%的同时,烟密度没有显著上升.对比EG、APP及EG/APP阻燃RPUF,体系残炭量越高、炭层耐热氧化能力越强,氧指数就越大;残炭表面越致密,产烟量就越少.添加EG/APP可显著降低含卤体系RPUF/TCPP的热释放、烟释放及CO释放速率,体现了EG与APP复合体系物理与化学膨胀结合的优势.  相似文献   

14.
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   

15.
A phosphorus-containing flame retardant, 4-(5,5-dimethyl-2-oxo-1,3,2-dioxaphosphorinan-2-yloxymethyl)-2,6,7-trioxa-1-phospha-bicyclo[2.2.2]octane-1-oxide (MOPO), was synthesized successfully and characterized. The flame retardancy and thermal behavior of a new intumescent flame-retardant (IFR) system for EVA, which was made of MOPO and ammonium polyphosphate (APP), were investigated by limiting oxygen index (LOI) test, vertical burning test (UL-94), cone calorimeter, and thermogravimetric analysis (TGA). An LOI value of 28.4 and UL-94 V-0 rating can be achieved when the total loading of MOPO and APP was 30 wt.%. The results from cone calorimeter indicate that both the heat release rate (HRR) and the total heat release (THR) of IFR-EVA decreased significantly compared with those of neat EVA. TG curves showed that the amount of residues increased significantly when intumescent additives were added; it also could be found that the LOI values increased with the increase in char residues. Meanwhile, morphology of the residues obtained from burning IFR-EVA in LOI test was studied through the SEM observations and rich compact char layers could explain the excellent flame retardance.  相似文献   

16.
以9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)、五硫化二磷(P2S5)为原料合成9,10-二氢-9-氧杂-10-磷杂菲-10-硫化物(DOPS),并将DOPS与聚磷酸铵(APP)组成复合阻燃剂,用于环氧树脂(EP)的阻燃改性.通过氧指数(LOI)、垂直燃烧(UL-94)、热失重(TGA)、锥形量热(CONE)和扫描电镜(SEM)等方法对改性后的环氧树脂的阻燃性能和阻燃机理进行了测试和分析.实验结果表明,DOPS/APP阻燃体系对EP具有很好的阻燃性能,且复配阻燃剂的阻燃效果比单一的阻燃剂阻燃效果好;其中,当阻燃剂的总添加量达到30%时即W_(DOPS)=10%、W_(APP)=20%时,阻燃EP复合材料的LOI值可达到29.2%,垂直燃烧等级达到UL-94 V-0级,残炭量可达49.3%.  相似文献   

17.
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   

18.
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   

19.
In order to solve the “candlewick effect” caused by glass fibers, which results in the decrease of flame retardancy of flame-retardant long-glass-fiber-reinforced polypropylene (LGFPP) systems, and the deterioration of mechanical properties caused by adding an additional amount of flame retardants compared with flame-retardant non-glass-fiber-reinforced polypropylene systems so as to keep a same flame retardancy, a novel intumescent flame retardant (IFR) system, which is composed of a charring agent (CA), ammonium polyphosphate (APP) and organically-modified montmorillonite (OMMT), was used to flame retard LGFPP. The thermal stability, combustion behavior, char formation, flame retardant mechanism and mechanical properties of the IFR-LGFPP samples were investigated by thermogravimetric analysis (TGA), limiting oxygen index (LOI), UL-94 test, cone calorimeter test, scanning electronic microscopy, and mechanical property tests. When the content of IFR is 20 wt%, the LOI value of IFR-LGFPP reaches 31.3, and the vertical burning test reaches UL-94 V-0 rating, solving the “candlewick effect” caused by long glass fiber without additional amount of the IFR. All the relevant cone calorimeter parameters also show that IFR-LGFPP has much better flame-retardant behaviors than LGFPP. Furthermore, the mechanical properties of IFR-LGFPP almost remain unchanged in comparison with those of LGFPP containing no IFR. The flame retardant mechanism was also discussed.  相似文献   

20.
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   

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