Preparation and properties of a single molecule intumescent flame retardant

Melamine salt of pentaerythriol phosphate (MPP), as a new single molecule intumescent flame-retardant, was prepared from pentaerythritol, phosphoric acid, and melamine, and then incorporated into polypropylene (PP) with organic montmorillonite (OMT) to obtain flame retardant PP/MPP/OMT composites. The flammability and combustion behavior of flame retardant PP composites were characterized by using LOI, UL-94 test, and cone calorimeter, respectively. The results showed that the flame retardant properties of the composite containing 29.0 wt% MPP and 1.0 wt% OMT are the best among all the composites. The digital photographs after cone calorimeter test demonstrated that moderate OMT could promote to form the homogenous and compact intumescent char layer.     

植酸三聚氰胺盐阻燃环氧树脂研究

利用生物基阻燃剂植酸三聚氰胺盐 (MPA) 阻燃改性环氧树脂并对其性能进行研究。通过红外光谱 (FTIR) 以及X射线光电子能谱 (XPS) 对MPA化学结构进行表征。利用热重分析仪 (TGA)、极限氧指数测试仪 (LOI)、垂直燃烧测试仪 (UL-94) 及锥形量热测试仪 (CC) 研究阻燃环氧树脂的热稳定性及阻燃性能。热重分析结果表明，MPA阻燃剂在800 ℃残炭达到25.6%，引入环氧树脂后可提升材料高温区热稳定性。垂直燃烧测试显示MPA在15%添加量下可赋予环氧树脂UL-94 V-0等级，表明MPA对环氧树脂有较好的阻燃效果。进一步锥形量热结果表明，MPA的加入显著降低了环氧树脂的热释放速率及总热释放，同时表现出优异的抑烟性能。     

抑烟剂对阻燃中纤板的燃烧性能影响研究

文章主要就抑烟剂对阻燃中纤板的燃烧性能影响进行了研究,最后研究出了一种低烟毒阻燃中纤板.经测试在阻燃剂添加量30 kg/m3情况下,当复合抑烟剂添加量2％时阻燃中纤板的氧指数为37.5％,UL94点燃续燃时间为3.5 s,阴燃时间为11.2 s,烟密度等级SDR由5.7下降到4.0.经GB8624-2012对阻燃中纤板进行燃烧性能测试,结果表明未发生火焰的横向、纵向蔓延,具有较好的阻燃、成炭性能.     

改性LDH与IFR对聚苯乙烯的协效阻燃研究

制备由聚磷酸铵（APP）、季戊四醇（PER）和十二烷基单磷酸钾改性的锌铝双氢氧化物（ZnAl-LDH-PK）组成的复合阻燃剂与膨胀阻燃剂IFR协效阻燃聚苯乙烯（PS）,研究了二者不同配比下对聚苯乙烯的阻燃性能、燃烧性能。结果表明,适当比例的ZnAl-LDH-PK和IFR协同作用于复合材料,可使材料具有更优异的热稳定性和成炭能力;当组分为PS、22%IFR、3%ZnAl-LDH-PK时,氧指数（LOI）达35,总热释放和生烟总量较纯PS分别降低了28%和38%,提高了耐火性能;SEM结果证实ZnAl-LDH-PK与IFR的协效作用使复合材料形成了高度膨胀和连续致密的炭层。     

Flame Retardance and Smoke Suppression of Poly(vinyl chloride) Using Multicomponent Systems

Metal-based organic complexes (MBO) are a class of FRSS additives that comprise a transition metal and an organic ligand that cleaves at an elevated temperature thereby releasing the metal in a reactive state. They help in the formation of char and thus act as an effective smoke suppressant. Use of MBO complexes as flame retardant smoke suppressants, phosphate ester as a flame retardant and active filler as endothermic material is reported here as multicomponent FRSS systems. MBOs used in the present study are the chelates of pentanediono. They were used alone as well as in combination with aluminum trihydrate (ATH) as filler were used to impart flame retardancy and smoke suppression to poly vinylchloride. Their performance was measured in terms of flammability, smoke generation, char formation and evolution of combustion gases. MBOs of molybdenum and chromium were found to be very efficient flame retardant smoke suppressants.     

Synergistic effects of inorganic tin compounds and Sb2O3 on thermal properties and flame retardancy of flexible poly(vinyl chloride)

The effects of inorganic tin compounds such as zinc hydroxystannate (ZHS), tin dioxide (SnO₂), and tin monoxide (SnO), Sb₂O₃, and their mixtures on the flame retardant and smoke suppressant properties of flexible poly(vinyl chloride) (PVC), and their flame retardant and smoke suppressant actions, were studied using the limiting oxygen index (LOI) test, the smoke density rating (SDR) test, thermogravimetric analysis/differential thermogravimetry/differential thermal analysis (TGA/DTG/DTA), scanning electron microscopy (SEM), and quantitative analysis. The results showed that the incorporation of small amounts of inorganic tin compounds and their mixtures with Sb₂O₃ can increase the LOI of PVC and decrease the SDR during combustion. Partial replacement of Sb₂O₃ in flexible PVC by ZHS resulted in a significant synergistic improvement in flame retardant behavior. TGA/DTG/DTA, SEM, and quantitative analysis showed that ZHS acts as a flame retardant in the solid phase, Zn²⁺ can catalyze dehydrochlorination of PVC and promote early cross-linking, leading to rapid charring, and Sn⁴⁺ can react with the char, thereby increasing the char stability. These actions, combined with the vapor-phase role of Sb₂O₃, can significantly enhance the flame retardancy of PVC.     

石墨烯微片对环氧树脂热性能的影响研究

研究石墨烯微片（GNS）对特种环氧树脂（AG-80/JD-919）的热稳定性和燃烧性能的影响。首先采用溶液共混法将GNS 添加到环氧树脂中,并利用热重分析仪（TGA）和锥形量热仪（CCT）分别对阻燃环氧树脂进行热稳定性和阻燃性能的测试分析。结果表明,GNS 添加量为6%时,环氧树脂的残炭量提高了4.6%,同时峰值热释放速率（pHRR）和总热释放量（THR）分别降低了40.63%和15.43%。因此,GNS 能够改善环氧树脂的热稳定性及其阻燃性能,这主要与GNS 在环氧树脂基体热分解过程能够起到物理阻隔作用有关。     

The Effect of Flame Retardant Smoke Suppressants on the Char Morphology of Plasticized PVC

Char formation that preserves the structural integrity of the polymer is one of the most efficient methods of reducing its flammability. Enhanced char formation from polymers such as PVC may also be associated with a decrease in smoke production, as is observed when the polymer is modified by a flame retardant smoke suppressant (FRSS) complex. A correlation had been made between the FRSS characteristics and char morphology. The effect of different flame retardant smoke suppressants on char formation has been highlighted.(UP)     

膨胀阻燃聚丙烯(PP)的燃烧、裂解及热化学性能研究

利用锥形量热仪、裂解气相色谱仪、示差扫描量热仪等分析测试手段，研究了PP及阻燃PP的对比性能。CONE的实验结果显示，阻燃剂的加入可显著降低PP的热释放速率，降低PP的各项燃烧性能参数指标；裂解图谱显示阻燃PP由于膨胀炭层的形成，降解速度明显减缓，相同条件下，降解组分浓度明显降低；热分析显示阻燃PP在升温过程中的放热量降低，耐热性明显增强。     

Synergistic effects of hydroxy silicone oil on intumescent flame retardant polypropylene system

The effects of hydroxy silicone oil (HSO) as a synergistic agent on the flame retardancy of intumescent flame retardant polypropylene composites (IFR-PP) were studied, and the IFR system mainly consisted of the ammonium polyphosphate (APP) and pentaerythritol (PER). The UL-94 test, thermogravimetric analysis (TGA), cone calorimeter (CONE), digital photograph and X-ray photoelectron spectroscopy (XPS) were used to evaluate the synergistic effects of hydroxy silicone oil. It has been found that the Polypropylene (PP) composite containing only APP and PER does not show good flame retardancy at 30% additive level. The cone calorimeter results show that the heat release rate, mass, total heat release, carbon monoxide and carbon dioxide of PP/APP/PER/HSO composites decrease in comparison with the PP/APP/PER ternary composite. The digital photographs demonstrated that HSO could promote to form the homogenous and compact intumescent char layer. Thus, a suitable amount of HSO plays a synergistic effect in the flame retardancy.     

阻燃沥青混合料阻燃抑烟性能及路用性能研究

设计沥青混合料直接燃烧试验,以试件燃烧时间、表面温度为指标评价阻燃剂对沥青混合料阻燃性能的影响;提出试件燃烧时烟雾面积的计算方法,以烟雾面积大小判别阻燃剂的抑烟效果;设计沥青混合料的路用性能试验,评价阻燃剂对沥青混合料路用性能的影响.结果表明:阻燃剂掺量越大,沥青的氧指数越高,沥青混合料试件的燃烧时间越短,表面温度越低,抑烟性能越好.阻燃效果较好的酸性阻燃剂会显著降低沥青混合料的高温稳定性和水稳定性.阻燃剂在沥青铺面工程中的适用性必须综合考虑其对沥青混合料阻燃性能和路用性能的影响.     

Enhanced flame retardancy of natural rubber composite with addition of microencapsulated ammonium polyphosphate and MCM-41 fillers

Microencapsulated ammonium polyphosphate with melamine-formaldehyde resin (MCMF-APP) prepared by in situ polymerization and characterized by FTIR showed decreased water solubility and particle size in comparison to bare ammonium polyphosphate. APP was used as additive to natural rubber (NR) together with mesoporous silica MCM-41 as a synergistic agent to form intumescent flame retardant composite in this study. The flame retardancies of NR/APP, NR/MCMF-APP and NR/MCMF-APP/MCM-41 composites were studied using limiting oxygen index (LOI) and UL-94 test, and their thermal stability was evaluated by thermogravimetric analysis (TGA) and dynamic mechanical thermal analysis (DMTA) as well as physico-mechanical properties. The results indicated that the LOI value of NR/MCMF-APP composite was higher than those of NR/APP composite and NR. Addition of MCM-41 into NR/MCMF-APP composite further increased the LOI values and also increased the UL-94 ratings of most ternary composites to V-0 due to a synergistic effect between MCM-41 and MCMF-APP in NR composites. As the results showed, the thermal stability and flame retardancy of NR were enhanced.     

壳聚糖/海藻酸钠涂层及其阻燃涤纶织物研究

以生物基多糖衍生的壳聚糖（CS）和海藻酸钠(AL)为改性剂,通过静电作用力驱动的层层自组装技术在聚对苯二甲酸乙二酯（PET）纤维织物进行阻燃修饰。通过扫描电镜,证实了壳聚糖和海藻酸钠在PET 织物表面的自组装沉积。利用热重分析仪与锥形量热仪等考察了壳聚糖和海藻酸钠的用量对PET 织物的热稳定性阻燃及抑烟性能的影响,并通过炭渣形貌和热解产物分析了天然生物基多糖的阻燃机理。结果表明,将生物基多糖沉积到PET 织物表面能有效提高织物的热稳定性、阻燃和抑烟性能。热解产物与炭层结构分析发现,天然生物基多糖的沉积促进了致密炭层的形成,有效地保护了底部聚合物,同时抑制了热解过程,从而提升了阻燃性能。     

Simplified structure of the condensed phase of fire retarded PA6 nanocomposites in TGA as related flammability

This paper concerns with the analysis of the nature of the mass residue of PA6 and its nanocomposites in nitrogen. To assess the structure of the condensed phase during pyrolysis, this study presents thermal (by TGA in nitrogen) and condensed phase analysis of the residue (by FTIR-ATR) of PA6 nanocomposites consisting of phosphorous based flame retardants (FR) and/or nanoparticles (based on modified Montmorillonite clay). The thermal analysis reveals that the nanoparticles do not change the pyrolysis kinetics of PA6 whereas the FR does. The FR and NC used in the polymer nanocomposites (PNC) are capable of changing the structure of the char compared with pure PA6, where the char structure consists of polycyclic aromatic hydrocarbons (PAH) whereas the PA6 does not leave any considerable amount of mass residue. This residue analysis for decomposition samples in TGA in Nitrogen of the PA6/FR/NC composites complements previously published work for gas phase analysis ( FTIR-gas) as well as cone calorimeter characterization for their flammability. The overall aim, addressed here also, is to find out to what extent microscale measurements (e.g. TGA/FTIR/DSC/ATR) can be used a priori to delineate the flammability of polymer fire retarded composites. It is shown that FTIR-gas and FTIR (ATR) residue can be used to determine the fire retardant action (solid and/or gaseous) only qualitatively.     

改性聚氨酯硬泡复合材料的阻燃性能研究

针对建筑保温材料所使用的硬质聚氨酯泡沫易燃的问题,对硬质聚氨酯泡沫进行化学接枝改性,使三聚氰胺基团均匀分散在阻燃材料体系中,通过对材料进行阻燃性能测试、力学性能测试、燃烧性能测试和扫描电镜分析,考察其在氢氧化镁/聚磷酸铵体系中的阻燃性能、压缩性能和抑烟性能。实验结果表明：三聚氰胺结构改性在对材料的压缩性能削弱较小的情况下可以大大提高纯聚氨酯材料的阻燃性能,不添加任何阻燃剂极限氧指数便可达26.4％,在氢氧化镁和聚磷酸铵协同阻燃体系中,极限氧指数可达28.4％,同时达到UL-94的V0等级。改性复合材料热释放速率最小可达到101.9 kW/m2,相较纯聚氨酯材料最大可下降35.3％,燃烧时产生的烟气释放速率相较纯聚氨酯最大可下降56.6％,并且形成致密的炭层,具有十分良好的阻燃效果。     

APP-DAP-CS膨胀阻燃体系阻燃聚甲醛研究

为提高聚甲醛(POM)的阻燃性能,以聚磷酸铵(APP)-磷酸氢二铵(DAP)-玉米淀粉(CS)为膨胀阻燃体系,将其与POM通过熔融共混制备了阻燃POM复合材料.并采用氧指数(LOI)仪、水平垂直燃烧(UL-94)测定仪、热重-差示扫描量热仪(TG-DSC)、扫描电镜(SEM)及锥形量热仪(CONE)等仪器对所制备的样品...     

Effects of aging on the properties of modified asphalt binder with flame retardants

Effects of aging on the properties of asphalt binders modified by incorporating Styrene–Butadiene–Styrene (SBS) and flame retardants (FR) were studied. Asphalt binders were artificially aged in the rolling thin film oven (RTFOT) and Pressure Aging Vessel (PAV). The flame retardancy of modified asphalt binders were characterized using limited oxygen index (LOI), and the effects of aging on the properties of asphalt binders were studied using Brookfield viscometer test and dynamic shear rheometer test. Experimental results indicated that the flame retardancy of asphalt binder was increased after aging. But the increasing amount of LOI is low when the modified asphalt binder containing more flame retardants. The variation of the LOI, softening point, penetration, ductility and viscosity of asphalt binder decreased with flame retardant content increasing, meaning the flame retardants can improve the thermo-oxidative aging resistance of asphalt binder. Furthermore, the G^*/sin δ, stiffness and m-value of flame retardant modified asphalt binders display smaller changes after two different aging.     

Effect of nitrogen phosphorus flame retardants on thermal degradation of wood

The effects of flame retardant action of wood treated with flame retardants that were obtained from phosphorus acid, pentaerythritol, urea, and triethanolamine through copolycondensation were studied in this research. Flame retardancy was characterized by limiting oxygen index (LOI), and the Broido method was used to evaluate the kinetics of thermal decomposition on untreated and treated wood. The effectiveness of these flame retardants was also investigated using scanning electron microscope (SEM) images of char formed after LOI tests. The results showed that adding the flame retardant decreases the thermal activation energy at a high degree of degradation, leading to the increase of LOI values. SEM images of chars showed the formation of protective polymeric coatings on char surfaces, and such coatings protected the substrate from damaging, resulting the integrity of wood fiber morphology and improvement of flame retardancy of wood during burning process.     

氮-磷协同阻燃聚氨酯保温材料性能研究

为了提高硬质聚氨酯的阻燃性能,采用磷改性聚醚,并添加三聚氰胺(Melamine)和聚磷酸胺(APP),并对试件的燃烧行为和热性能进行了研究。结果表明:在含磷硬质聚氨酯保温隔热材料中等比例添加Melamine和APP,能形成氮-磷协同阻燃体系,材料的阻燃性能得到显著提高,其中氧指数达34.43%,水平燃烧等级达到FH-1,垂直燃烧等达FV-0。     

CS/h-BN/APP层层自组装涂层阻燃杨木的研究

为提高杨木的阻燃性能,利用带正电性的壳聚糖/六方氮化硼(CS/h-BN)聚电解质溶液,以及带负电性的聚磷酸铵(APP)溶液,基于层层自组装(LBL)技术,通过两聚电解质溶液之间的静电吸附作用,在木材表面成功制备出具有良好阻燃性能的CS/h-BN/APP薄膜涂层.结果表明:所制备的涂层均匀分布在木材表面,且具有良好的附着力;涂层阻燃木材试件的热释放速率、烟释放速率显著降低,第2放热峰出现时间晚于未处理木材试件,且在燃烧过程中的残余物质量始终高于未处理木材试件,完全燃尽时间则比未处理木材试件多出约100s,阻燃效果随着自组装涂层数的增加而逐渐增强;涂层阻燃木材试件的CO、CO_2气体生成量明显降低,表明阻燃涂层能有效降低木材烟气及毒性气体释放;涂层阻燃木材试件较未处理木材试件更好地保持了木材本身的结构,显示出了良好的抵抗火灾能力.