Studies on the effect of different levels of toughener and flame retardants on thermal stability of epoxy resin

A thermoplastic toughener, polyether sulphone (PES) and a number of different types of flame retardants were blended in different ratios with a commercial epoxy resin triglycidyl-p-aminophenol (TGAP) and 4,4-diamino diphenyl sulphone (DDS) a curing agent. The effect of type and levels of flame retardants (FR) and the toughening agent on the curing, thermal decomposition and char oxidation behaviour of the epoxy resin was studied by the simultaneous differential thermal analysis and thermogravimetric techniques. It was observed that the toughener slightly increases the curing temperature (by up to 20 °C) but had minimal effect on the decomposition temperature of the resin. Flame retardants, however affected all stages depending upon the type of flame retardant used. The curing peak for samples containing tougher and flame retardants although slightly changed depending upon the type of FR, was not more than ± 20 °C compared to that of samples containing toughener only. All flame retardants lowered the decomposition temperature of the epoxy resin. Phosphorus- and nitrogen-containing flame retardants reduced the char oxidation leading to more residual char, whereas halogen- containing flame retardants had less effect on this stage.     

Influence of oxidation state of phosphorus on the thermal and flammability of polyurea and epoxy resin

The focus of this study is an investigation of the effect of oxidation state of phosphorus in phosphorus-based flame retardants on the thermal and flame retardant properties of polyurea and epoxy resin. Three different oxidation states of phosphorus (phosphite, phosphate and phosphine oxide) additives, with different thermal stabilities at a constant phosphorus content (1.5 wt.%) have been utilized. Thermal and flame retardant properties were studied by TGA and cone calorimetry, respectively. The thermal stability of both polymers decreases upon the incorporation of phosphorus flame retardants irrespective of oxidation state and a greater amount of residue was observed in the case of phosphite. Phosphate was found to be better flame retardant in polyurea, whereas phosphite is suitable for epoxy resin. Phosphite will react with epoxy resin by trans-esterification, which is demonstrated by FTIR and ³¹P NMR. Further, TG–FTIR and XPS studies also provide information on flame retardancy of both polymers with phosphorus flame retardants.     

Smoke and hydrocarbon yields from fire retarded polymer nanocomposites

Polypropylene (PP) and Polyamide 6 (PA6) samples, with and without fire retardants (FR) (ammonium polyphosphate in PP, and a mixture of organic aluminium phosphinate and melamine polyphosphate (OP 1311) in PA 6) and nanofillers (NC) were burned under different fire conditions in order to compare their toxic product yields. Fire effluents (CO, smoke and hydrocarbons) were generated using a steady state tube furnace (BS 7900, ISO TS 19700) for the separate materials and fire retarded and nanocomposite modifications of these materials under flaming conditions. Under well-ventilated conditions yields of carbon monoxide (CO) for all PP samples are similar, whereas for PA6 samples much higher yields of CO for PA6 + FR and PA6 + NC are observed. The highest yields of CO occur for both pure polymers in under-ventilated fire conditions when fire retardant and nanoclay are combined together. For PP the smoke is fairly independent of fire condition, but the PP + FR + NC shows less agglomeration. For PA6 the sample containing OP 1311 shows consistently higher smoke yields. For hydrocarbon yields similar effects are observed for both PP and PA6 polymers; the highest yields are for PA6 + NC, except under-ventilated fires where PA6 + FR produce the most; for PA6 + FR + NC samples the lowest yields are observed, compared to either NC or FR formulations.     

A review on potential development of flame retardant kenaf fibers reinforced polymer composites

Kenaf fibers have been extensively explored from the past few decades in polymer composites industries owing to its extensive adaptations, excellent properties together with its comparable mechanical properties to traditional glass fibers polymer composites. The combustibility or lowered flame retardancy hampered the diverse applications of kenaf fibers reinforced polymer composites, as it affects the mechanical strength and stiffness of composites during fire. Current review article intended to be a comprehensive source of published literature involving the flame retardants (FRs), types and applications of FRs and the fabrication of kenaf fibers reinforced polymer composites. This article will also provide a perfect data on the recent development of the FR kenaf fibers polymer composites with different FRs and explored its structural and semi‐structural industrial application for performing further research in this topic. Copyright © 2016 John Wiley & Sons, Ltd.     

Investigation of the flammability of different textile fabrics using micro-scale combustion calorimetry

Evaluating and analyzing the performance of flame retardant (FR) textiles are a critical part of research and development of new FR textiles products by the industry. The testing methods currently used in the industry have significant limitations. Most analytical and testing techniques are not able to measure heat release rate (HRR), the single most important parameter in evaluating the fire hazard of materials. It is difficult to measure HRR of textile fabrics using cone calorimetry because textile fabrics are dimensionally thin samples. The recently developed micro-scale combustion calorimetry (MCC) is able to measure the following flammability parameters for textile using milligram sample sizes: heat release capacity, HRR, temperature at peak heat release rate (PHRR), total heat release and char yield. In this research, we applied MCC to evaluate the flammability of different textile fabrics including cotton, rayon, cellulose acetate, silk, nylon, polyester, polypropylene, acrylic fibers, Nomex and Kevlar. We also studied the cotton fabrics treated with different flame retardants. We found that MCC is able to differentiate small differences in flammability of textile materials treated with flame retardants. We were also be able to calculate the limiting oxygen index (LOI) using the thermal combustion properties of various textile samples measured by the MCC. The calculated LOI data have yielded good agreement with experimental LOI results. Thus, we conclude that MCC is an effective new analytical technique for measuring textile flammability and has great potentials in the research and development of new flame retardants for textiles.     

PA‐6 and EVA alloy/clay nanocomposites as char forming agents in poly(propylene) intumescent formulations

This study investigates the influence of nylon‐6 (PA‐6) and ethylene‐vinyl acetate copolymer (EVA) alloy/clay nanocomposites on the properties of the flame‐retardant (FR) poly(propylene). Cone calorimetry and scanning electron microscopy (SEM) techniques were used to investigate the effect of PA‐6 and EVA alloy nanocomposites on the fire properties and dispersion of intumescent flame‐retardants (IFRs). The experimental results show that PA‐6 and EVA alloy nanocomposites improve the fire and mechanical properties of the FR poly(propylene). It is also shown that the improvement of the properties mainly depends on the weight ratio of PA‐6 and EVA in the alloys. The probable mechanisms are discussed in this paper. Copyright © 2005 John Wiley & Sons, Ltd.     

A study of fire retardant blooming in HIPS by molecular modeling

The blooming process of two fire retardants: FR 1808 (by DSBG) and FR 8010 (by Albemarle) in high impact polystyrene (HIPS) was studied using experimental and computational methods. The degree of blooming was determined by accelerated aging followed by transmission electron microscopy (TEM) micrographs. Several levels of computational tools were used. On the molecular level, forced diffusion, calculations showed that the relative diffusion coefficient of FR 1808 in pure polystyrene (PS) is significantly higher than that of FR 8010. It was shown that this diffusion coefficient could be reduced by the addition of chloroprene and polychloroprene. Cohesive energy density (CED) solubility parameter and heat of mixing calculations showed that FR 1808 was compatible in PS, with an even higher compatibility in the interface of PS and butadiene in HIPS. TEM micrographs were in agreement with these findings. A three‐stage blooming mechanism was suggested: FR 1808 accumulates in the PS butadiene interface and diffuses to the surface, through the butadiene inclusions, due to FR 1808 concentration gradient. Copyright © 2010 John Wiley & Sons, Ltd.     

界面聚合法制备正二十烷微胶囊化相变储热材料

采用界面聚合的方法, 以甲苯鄄2,4-二异氰酸酯(TDI)和乙二胺(EDA)为反应单体, 非离子表面活性剂聚乙二醇壬基苯基醚(OP)为乳化剂, 合成了正二十烷为相变材料的聚脲包覆微胶囊. 结果表明, 二异氰酸酯和乙二胺按质量比1.9:1 进行反应. 以透射电镜和激光粒度分析仪分析微胶囊, 测得空心微胶囊直径约为0.2 μm, 含正二十烷微胶囊约为2-6 μm. 红外光谱分析证明, 壁材料聚脲是由TDI 及EDA 两种单体形成的. 正二十烷的包裹效率约为75%. 微胶囊的熔点接近囊芯二十烷的熔点, 而其储热量在壁材固定时随囊芯的量而变. 热重分析表明, 囊芯正二十烷、含正二十烷的微胶囊以及壁材料聚脲, 能够耐受的温度分别约为130 ℃、170 ℃及270 ℃.     

A Study of the Slow Release of Urea from Microcapsules with TDI as the Wall-Sealing Treatment

The release of urea from ethylcellulose coated microcapsules was efficiently reduced by post-treatment with toluene-2,4-diisocyanate (TDI) in n-hexane. Our results show that TDI can be used as a sealant which modifies the shell characteristics of the ethylcellulose film. The modification is rather complicated in that it probably includes cross-linking between ethylcellulose and TDI, a reaction between urea and TDI, and biuret or polyurea formation from TDI absorbed on the microcapsules surface with moisture. The influence of post-treated conditions on the release of urea from ethylcellulose shell was studied.     

Effects of microparticles on isotactic polypropylene: Thermomechanical and thermal properties

Five types of melamine-formaldehyde microcapsules, that is, with shells of different compositions [melamine formaldehyde shell or a melamine formaldehyde-poly(hexamethylene adipate glycol) shell] and containing or not a flame retardant, diammonium hydrogen phosphate (DAHP), have been prepared by an in situ polymerization method and have been added to an isotactic polypropylene matrix (iPP) by melt blending at 5 wt %. Wide-angle X-ray diffraction and differential scanning calorimetry were employed to investigate the crystallization behavior of the prepared iPP/microparticles composites. The tensile properties and the thermal stability were also evaluated. It was stated that the morphology and the shape of the microparticles not only influence the crystallization behavior but also the thermomechanical properties of these composites. Thus, rougher microparticles act as a nucleating agent for the iPP, and in the presence of microparticles containing DAHP, the α- and the β-crystals are formed. Moreover, the presence of microparticles improves the thermal stability of the iPP. © 2008 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 46: 2566–2576, 2008     

Effect of Organo‐Modified Nanosepiolite on Fire Behaviors and Mechanical Performance of Polypropylene Composites

The objective of the study was to investigate the effect of the organo‐modified nanosepiolite (ONSep) on improving the fire safety of polypropylene (PP). The composites based on PP, flame retardant master batch (MB‐FR, 25 wt% PP+50 wt% decabromodiphenyl ether (DBDPE)+25% antimony trioxide (ATO)) and ONSep were prepared via melt blending. The results of the limiting oxygen index (LOI) and vertical burning rating (UL‐94) test indicated that PP/40 wt% MB composites had no rating with seriously dripping phenomenon, while the LOI value was only 22.5. However, as 4 wt% ONSep was added in PP/40 wt% MB composites, the composites achieved UL94 V‐0 rating and the LOI value was 24.3. In comparison, PP/50 wt% MB composites could not reach the V‐0 rating either. The TGA results revealed that the addition of ONSep enhanced the thermal stability of the PP/MB‐FR composites. The cone calorimeter results indicated that the heat release rate, average mass loss rate, smoke production rate and smoke temperature of the PP/40 wt% MB‐FR/4 wt% ONSep composites decreased in comparison with those of PP/40 wt% MB‐FR composites. Simultaneously, the Young modulus and impact strength were also much better improved with the increase of ONSep loading. Therefore, the synergistic flame retardancy of ONSep in PP/MB‐FR matrix significantly containing a halogen based flame retardant (DBDPE) significantly improved the fire safety and mechanical properties of the composites, and allowed to decrease the total amount of brominated fire retardants.     

正十六烷聚脲微胶囊化相变材料

用界面聚合法，合成了直径大约2.5 μm可用于热能储存含相变材料的聚脲包覆微胶囊.在含乳化剂的水溶液中，将溶有芯材正十六烷的有机相乳化成微米级油性液滴，随后加入的水溶性单体二胺与甲苯2,4-二异氰酸酯在胶束界面相互反应形成囊壁.分别用乙烯二胺，1,6-己二胺和它们的混合物作为水溶性单体进行了研究.并用红外光谱和热分析分别考察了不同胺类对微胶囊化学结构和热性质的影响.红外谱图显示合成了聚脲微胶囊，热重曲线表明含正十六烷的聚脲微胶囊能够耐受大约300 ℃高温，差示扫描量热测试表明所有样品均具有合适的相转变热，冷热循环实验揭示微胶囊能够维持储热容量不衰减.研究表明微胶囊化的正十六烷作为相变储热材料具有良好的应用前景.     

阻燃聚丙烯共混体系结晶形态研究

本工作利用WAXD、DSC、PLM、PCM和SAIS等手段,对几种具有代表性的阻燃PP共混体系的结晶形态和结晶行为进行了研究。结果表明各种阻燃剂存在,对阻燃PP体系中PP的结晶形态和结晶行为有明显影响。其影响情况取决于这些阻燃剂自身的各种特性。另外,PP的结晶对某些阻燃剂的分散也有一定的影响,其结晶过程是体系中阻燃剂的一个再分散过程。     

Formation of Pickering emulsion by use of PCM and SiC and application to preparation of hybrid microcapsules with interfacial polycondensation reaction

It was tried to form Pickering emulsion by use of paraffin wax as a phase change material (PCM) and SiC as solid powder and to apply to the preparation of the hybrid microcapsules with the interfacial polycondensation reaction. Pickering emulsion could be formed by stirring PCM and SiC in the continuous water phase. The mean diameter of PCM droplets in the (O/W) emulsion decreased with the added amount of SiC. The SiC weight adhered on the surface of PCM droplets become the maximum in the continuous phase with pH 6.8. The hybrid microcapsules with the shell made of SiC and polyurea resin film could be prepared by using Pickering emulsion. There was a critical adhesion weight of SiC, above which the hybrid microcapsules could not be formed. Thermal conductivity of hybrid microcapsules could be improved as compared with the PCM microcapsules. Copyright © 2015 John Wiley & Sons, Ltd.     

Encapsulation of palladium in polyurea microcapsules

An interfacial polymerisation approach is adopted to encapsulate palladium(II) acetate and palladium nanoparticles in polyurea microcapsules for use in catalysis.     

阻燃剂对5Ah锂离子软包电池倍率性能和安全性能的影响研究

在电解液中加入不同含量(5 %,10 %,20 %)的阻燃剂,研究了其对LiNi _0.4Co_0.2Mn_0.4 O₂三元材料作为正极材料组装的5 Ah锂离子软包电池的倍率性能、过充性能和短路性能的影响. 实验结果表明,电解液中5 %体积含量的阻燃剂使软包电池在1C和2C放电时,具有最好的倍率性能;当阻燃剂的体积含量提升到20 %,在过充时,电池表面温度升高的最少;在短路实验时,电池不起火、不爆炸.     

Microencapsulation of osmium tetroxide in polyurea

[reaction: see text] Osmium tetroxide has been microencapsulated in a polyurea matrix using an in situ interfacial polymerization approach. These microcapsules have been effectively used as recoverable and reusable catalysts in the dihydroxylation of olefins     

Preparation of microcapsulated ammonium polyphosphate,pentaerythritol with glycidyl methacrylate,butyl methacrylate and their synergistic flame‐ retardancy for ethylene vinyl acetate copolymer

A new series of microcapsules containing pentaerythritol (PER) and ammonium polyphosphate (APP) with glycidyl methacrylate and butyl methacrylate as shell materials were synthesized by in situ polymerization. The structure and performance of the microencapsulated APP and microencapsulated PER were characterized by Fourier transform infrared spectroscopy, X‐ray photoelectron spectroscopy, scanning electron microscopy, and water contact angle. The flame retarded ethylene‐vinyl acetate copolymer (EVA) composites were studied by limiting oxygen index, UL‐94 test, and cone calorimeter. It was found that the microencapsulation of flame retardants (FRs) with the glycidyl methacrylate and butyl methacrylate lead to a decrease in the particle's water solubility and an improvement of the hydrophobicity. Results also demonstrated that the FR properties of EVA/microencapsulated APP/microencapsulated PER composites were better than those of the EVA/APP/PER composites at the same loading of FRs. The thermogravimetric analysis results reflected that the microencapsulated EVA composites had better thermal stability because of the forming of stable char during the combustion. Copyright © 2013 John Wiley & Sons, Ltd.     

Development of additives possessing both solid-phase and gas-phase flame retardant activities

Effective additives are required to impart a measure of fire retardancy to polymeric materials used in a variety of applications. Traditionally, these have been gas-phase active additives, most commonly organohalogen compounds or solid-phase active agents, often organophosphorus compounds. Organosphosphorus flame retardants are often very effective but may suffer from a cost disadvantage when compared with their organobromine counterparts. Organohalogen flame retardants are usually quite effective but their use is a subject to several environmental concerns. The development of additives that could simultaneously promote both types of fire retardant action could make available flame retardants that are both more cost effective and more environmentally friendly than those currently in use. Several sets of compounds with the potential to display both solid-phase and gas-phase flame retardant activities have been prepared and evaluated.     

Synthesis and Characterization of Microcapsules with Chlorpyrifos Cores and Polyurea Walls

Microcapsules with chlorpyrifos cores and polyurea walls were synthesized with 2,4-tolylene diisocyanate as an oil-soluble monomer and ethylenediamine as a water-soluble monomer via an interracial polycondensation reaction. The products were characterized by means of Fourier transform infrared spectrometry, ^13C NMR spectrometry and ^31p NMR spectrometry. The morphology, the particle size and the particle size distribution, and the thermal properties were also evaluated. The prepared microcapsules exhibit clear and smooth surfaces and have a mean diameter of 28. 13 μm. These microcapsules also have a good thermal stability for long-term use, and have potential applications in minimizing the toxicity of chlorpyrifos through controlled release.