环氧树脂/甲基环己基次膦酸铝阻燃复合材料性能研究

以甲基环己基次膦酸铝(AMHP)作为环氧树脂(EP)的阻燃剂,着重研究了AMHP对EP/ AMHP阻燃复合材料的阻燃性能、力学性能及热稳定性能的影响。结果表明,添加15 %(质量分数,下同) 的AMHP就可以使阻燃复合材料的极限氧指数达到28.6 %,UL 94测试达到V-0级标准,700 ℃时的残炭率为16.34 %,玻璃化转变温度（Tg）明显提高;随着AMHP的加入,阻燃复合材料的冲击强度降低,弯曲强度和弯曲模量略有下降。     

气相二氧化硅对环氧树脂的辅助阻燃作用

将气相Si O2与含膦阻燃剂复配,应用到环氧树脂(EP)中,着重研究了该复合材料的阻燃性能、热分解性能及玻璃化转变温度(Tg),结果表明当气相Si O2含量为3%时,复合材料的氧指数值达到28.3%,垂直燃烧通过UL94 V-0标准。在热分解过程中,各组分之间相互作用,复合材料的玻璃化转变温度比纯EP的要高,残炭率也增加。可见气相Si O2起到一定的辅助阻燃作用。     

纳米Al_2O_3对含磷环氧树脂体系的性能影响

研究了以纳米Al_2O_3作为协同阻燃剂,对EP/DOPO和EP/HPCTP树脂固化物阻燃性能的影响。通过热重分析测试(TGA)、动态热机械分析测试(DMA)、氧指数测定(LOI)及垂直燃烧测试(UL-94)重点探讨了树脂固化物的耐热及阻燃性能。测试结果表明,含磷阻燃剂有助于提高环氧树脂固化物的阻燃性能,但会降低其玻璃化转变温度(Tg)。随着纳米Al_2O_3的加入,残炭率(800℃)、极限氧指数(LOI)得到进一步的提高,并且能够在一定程度上提升树脂固化物的玻璃化转变温度(Tg)和初始热裂解温度(T5%)。     

环氧树脂/有机化蒙脱土纳米复合材料的研究

采用插层原位聚合法制备了环氧树脂/有机化蒙脱土(EP/OMMT)纳米复合材料,探讨了OMMT的剥离结构及其对EP/OMMT纳米复合材料热性能和力学性能等影响。结果表明:当w(OMMT)=7%时,EP/OMMT纳米复合材料的热变形温度提高了24～27℃,Tg(玻璃化转变温度)提高了20～30℃,并且其力学性能和耐湿热性能均优于纯EP体系。     

PEPA阻燃环氧树脂的性能研究

将反应型含磷阻燃剂1-氧代-4-羟甲基-2,6,7-三氧杂-1-磷杂双环[2.2.2]辛烷(PEPA)与环氧树脂(EP)反应制得含磷EP,经固化剂间苯二胺固化后得到阻燃EP.表征了阻燃EP的热稳定性、成炭性和阻燃性能等.结果显示,PEPA的羟基与EP的环氧基团发生反应,使EP环氧当量提高.随着PEPA含量增加,阻燃EP的氧指数逐渐增大,起始分解温度降低,最终质量保持率增大.PEPA的加入对阻燃EP的玻璃化转变温度影响不大.燃烧后形成的炭层表面结构致密,内部多孔.     

新型反应型磷-氮阻燃剂的合成与应用

采用膦酸酐和苯胺为原料,通过一步法合成了一种含N-P的具有反应活性的β-（N-苯基酰胺）乙基甲基次膦酸(CEMP),通过FTIR和1H-NMR对其结构进行了表征。初步探讨了CEMP在环氧树脂(EP)中的应用。结果表明:CEMP是一种有效的EP阻燃剂,当阻燃剂添加量为20 %(质量分数,下同)时即可满足UL94-V0的阻燃等级,极限氧指数达到29.4 %,弯曲强度比未阻燃的EP有了较大的提高,但玻璃化转变温度（Tg)）有所下降。     

DDS固化EP/MMT纳米复合材料性能研究

以4,4′-二氨基二苯砜(DDS)为固化剂,制备出一种剥离型MMT/EP(蒙脱土/环氧树脂)纳米复合材料。采用红外光谱(FT-IR)法、X射线衍射(XRD)法和动态力学分析(DMA)法等对复合材料的微观结构、插层剥离行为、热性能和力学性能等进行了研究。结果表明:MMT对EP分子结构无影响,有利于EP结构和性能的设计,也便于确定其固化工艺。在无促进剂的情况下,当体系中引入5%MMT(相对于EP质量而言)时,复合材料的干态热变形温度、玻璃化转变温度(Tg)、冲击强度和拉伸强度分别提高了39℃、21℃、27.30%和10.50%;适量的MMT能有效提高纳米复合材料的耐湿热性能。     

POP-290阻燃剂对丙烯酸酯光固化涂料的影响

制备了双酚A环氧丙烯酸酯(EA)/阻燃剂(POP-290,聚合物聚醚多元醇)/活性单体阻燃UV涂料,主要考察了不同用量的阻燃剂对丙烯酸酯UV涂料的阻燃性能和光固化的影响.研究结果表明,阻燃剂的使用提高了UV涂料体系的固化速度、凝胶含量及玻璃化转变温度(Tg).当m(EA)∶m(活性单体)=4∶1,POP-290含量为7%(质量分数)时,水平燃烧等级达到FH-1,LOI从原来的21提高到26.     

阻燃香蕉纤维增强环氧树脂复合材料的动态力学性能和热性能研究

采用硅烷偶联剂(A-174)对香蕉纤维(BF)进行表面处理,采用硫酸铵、硼砂、磷酸氢二铵、磷酸三丁酯作为阻燃剂处理BF,选用添加了阻燃剂三聚氰胺焦磷酸盐(MPP)和季戊四醇(PER)的环氧树脂作为基体树脂,通过热压成型工艺制备阻燃BF增强环氧树脂复合材料。分别采用动态力学分析(DMA)、扫描电镜(SEM)、热重分析(TG)研究阻燃BF增强环氧树脂复合材料的动态力学性能、微观形貌以及热性能。结果表明:当阻燃BF含量为30%时,复合材料的储能模量、损耗模量达到最大值,分别比纯环氧树脂提高了570%和110%;当阻燃纤维含量为20%时,复合材料的玻璃化转变温度也比纯环氧树脂提高了16.9℃。通过扫描电子显微镜(SEM)观察说明纤维与环氧树脂之间产生良好的界面黏合作用,宏观上表现为动态力学性能的提高;热失重研究结果表明,阻燃BF的加入能明显提高环氧树脂的热分解温度和残炭率。     

EP/GNs/MWCNTs复合材料的导热性能

以多壁碳纳米管(MWCNTs)和石墨烯纳米微片(GNs)为导热填料,环氧树脂(EP)为基体采用溶剂和超声分散法,制备了EP/GNs/MWCNTs导热复合材料,并与EP/MWCNTs及EP/GNs复合材料的导热性能进行了对比。采用透射电子显微镜观察其微观结构,采用Hot Disk热导率测试仪测试其导热性能,采用差示扫描量热法和热重分析仪测试其耐热性及热稳定性。结果表明,MWCNTs和GNs共同作为EP导热填料时,相比于单组分填料(MWCNTs或GNs)更易形成导热网络;EP的热导率、玻璃化转变温度(Tg)和热分解温度均随着MWCNTs或GNs含量的增加而提高,其中,GNs更有利于提高EP的热导率和热分解温度,MWCNTs更有利于提高EP的Tg。在相同的导热填料含量下,相对于其中的任一单一填料,MWCNTs/GNs共同作用时,对热导率的提高有更显著的效果,且随着其中GNs比例的增加,热导率逐渐增大。当GNs和MWCNTs的体积分数分别为0.6%和0.4%时,EP/GNs/MWCNTs复合材料的热导率、Tg和起始分解温度分别为0.565 W/(m·K),152℃和316℃,分别比纯EP提高了132.5%,34.5%和8.2%。     

EP/MOC复合材料热分解动力学与阻燃性能研究

采用Kissinger法和Crane法对环氧树脂/氯氧镁(EP/MOC)阻燃复合材料在空气中不同升温速率下的热重(TG)和差热(DTA)曲线进行了热解动力学研究。测定了EP/MOC复合材料中EP起始分解和终止分解放热峰的特征温度。结果表明:EP/MOC复合材料中的EP活化能高于纯EP,说明MOC增强了EP的热稳定性,提高了热解温度;EP/MOC中的EP热分解反应级数和纯EP基本相同,说明同条件下的EP和MOC对热分解速率的影响是相同的;另外,该EP/MOC复合材料具有良好的阻燃性能。     

Comparative study of aluminum diethylphosphinate and aluminum methylethylphosphinate‐filled epoxy flame‐retardant composites

Epoxy resin (EP) is one of the main polymers in electrical and electronic applications. In this work, flame‐retardant epoxy resin composites based on aluminum diethylphosphinate (Al(DEP)) and aluminum methylethylphosphinate (Al(MEP) were prepared using aromatic amine 4, 4‐diaminodiphenylmethane as curing agent. The flammability, thermal degradation, flexural properties, and morphologies of composites were investigated with respect to the filler loading and filler type. Results showed that both Al(MEP) and Al(DEP) were efficient flame retardants for EP and a low dosage (15 wt%) is enough to achieve the important criterion UL 94 V‐0. Limiting oxygen index (LOI) of composites is increased with filler loading (phosphorus content) and reached of 32.2% for 15 wt% of Al(MEP) and 29.8 for 15 wt% of Al(DEP). The char formation and flexural modulus of composites are also improved by adding the two fillers. However, the flexural strength of all the composites decreased with increasing filler loading. In comparison with Al(DEP)/EP, Al(MEP)/EP provides a higher flammability, better thermal stability and char formation but inferior flexural properties. Scanning electron microscopy revealed that the dispersion of Al(DEP) filler in the EP matrix is more uniform and exhibits better compatibility with EP matrix, which in turn generates better flexural strength and higher modulus when compared with Al(MEP)‐filled EP composites. POLYM. COMPOS., 2012. © 2012 Society of Plastics Engineers     

纳米Sb_2O_3/环氧复合材料阻燃耐热及力学性能研究

通过氧指数、力学性能测定及热重分析研究了纳米Sb2O3与十溴二苯醚(FR-10)配合使用时,纳米Sb2O3/环氧树脂复合材料的阻燃性、耐热性和力学性能,并与微米Sb2O3/环氧树脂体系进行了对比。结果表明,Sb2O3与FR-10共用时对环氧树脂具有明显的协同阻燃作用,Sb2O3的加入抑制了环氧树脂固化物的热分解;添加少量的Sb2O3就能达到较好的阻燃效果。加入纳米Sb2O3后材料的拉伸强度、弯曲强度和冲击强度均有提高。添加纳米级Sb2O3时体系阻燃、耐热和力学性能明显好于微米级Sb2O3填充体系。     

Al（OH）3和Mg（OH）2阻燃EVA性能的研究

选用形貌、粒径尺寸及分布相近的两种无机阻燃剂氢氧化铝（Al（OH）3）和氢氧化镁（Mg（OH）2），研究了二者用量对乙烯-醋酸乙烯酯共聚物（EVA）复合材料的力学性能和阻燃性能的影响，并比较了添加红磷的复合材料的力学性能和阻燃性能。研究表明：Al（OH）3和Mg（OH）2用量对复合材料性能影响比较相似，随着阻燃剂用量的增加，复合材料的阻燃性能提高，拉伸强度增加，但断裂伸长率下降；通过锥形量热仪数据看出：Al（OH），的点燃时间短，最大热释放速率和平均热释放速率低，火行为指数大，阻燃效果比Mg（OH）2好；红磷的加入对复合材料力学性能影响不大，而对阻燃性能影响较大。Mg（OH）2与红磷复配能提高复合材料的氧指数，但是，从水平和垂直燃烧角度考虑，Al（OH）3与红磷之间的阻燃协效效果更好。     

聚醚醚酮/多壁碳纳米管复合材料力学及阻燃性能研究

通过熔融共混法将聚醚醚酮（PEEK）与多壁碳纳米管(MWCNT)混合,利用模压法制备了MWCNT增强型PEEK复合材料,研究了MWCNT对PEEK性能的影响。结果表明,添加一定比例的MWCNT能够提高PEEK的力学和阻燃性能;当MWCNT含量为5%（质量分数,下同）时,PEEK的弯曲强度提高了53%;当MWCNT含量为1%时,锥形量热法测得的热释放速率峰值最低,燃烧性能指数值最大,热重分析显示初始分解温度较纯PEEK提高了13℃,表明MWCNT有效地提高了PEEK的阻燃和热稳定性能。     

丁腈橡胶/疏松型纳米氢氧化镁复合材料的性能

用气泡液膜法(GBLM)制备的疏松型纳米氢氧化镁(LN-MH)填充丁腈橡胶(NBR),研究了复合材料的阻燃性能、力学性能、抽提率、门尼黏度及交联密度。结果表明,随着LN-MH用量的增加,LN-MH对NBR具有显著的纳米增强作用,改善了复合材料的阻燃性能、力学性能、门尼黏度和交联密度,但对复合材料在甲苯中的抽提率无影响。     

Synthesis of aluminum ethylphenylphosphinate flame retardant and its application in epoxy resin

A novel flame retardant additive, aluminum ethylphenylphosphinate (AEPP), was synthesized from diethyl phenylphosphonite and aluminum chloride hexahydrate, and characterized by FTIR, ¹H NMR, and ³¹P NMR. AEPP was added into diglycidyl ether of bisphenol A epoxy resin (EP) cured by bisphenol A‐formaldehyde novolac resin. The flame retardancy of the cured EP was investigated by limited oxygen index, UL 94 test, and cone calorimeter test. The results revealed that the EP composite containing 15% AEPP had a limited oxygen index value of 28.2% with a UL 94 V‐0 rating. The incorporation of AEPP effectively decreased the peak heat release rate and the total heat release in cone calorimeter test analysis. Scanning electron microscopy results showed that the introduction of AEPP benefited to the formation of a smooth and continuous char layer during combustion of the flame retarded EP. The thermogravimetric analysis results indicated that the incorporation of AEPP promoted the initial decomposition of EP matrix, but AEPP/EP composites had a higher char yield at high temperatures. Moreover, the flexural properties of the flame retarded EP composites were studied.     

无卤阻燃SBR的阻燃性能及热失重行为

利用锥形量热仪(CONE)和热失重分析(TG)研究了化学膨胀阻燃剂(IFR)、氢氧化铝/红磷(Al(OH)3/P)及二者复合阻燃SBR的阻燃性能及热失重行为。结果表明,阻燃剂用量为40份,聚磷酸铵(APP)与季戊四醇(PER)质量比为3∶1时,SBR/APP/PER的热释放速率及生烟速率均大幅度下降,阻燃效果较好;Al(OH)3与P质量比为26∶14时,可有效降低SBR/Al(OH)3/P的热释放速率,但生烟速率较大;将APP/PER∶Al(OH)3/P=1∶1复配,SBR/IFR/Al(OH)3/P的热释放速率和生烟速率没有进一步改善,协同效应不明显。热失重研究表明,空气气氛下,试样SBR/IFR/Al(OH)3/P在300~500℃时,Al(OH)3/P反应使得SBR分解速度下降;在500~800℃时,APP与PER形成炭层,有效地起到隔热隔氧的作用,从而抑制炭黑的分解;两者复合使用,使阻燃SBR分解速度降低,热稳定性提高。     

无卤阻燃永久抗静电GFPP材料研制

以玻纤增强聚丙烯(GFPP)为基体,加入无卤阻燃剂FR–1420、永久抗静电剂P–22制备复合材料,考察了体系的阻燃性能、永久抗静电性能、力学性能和热稳定性能.结果表明,FR–1420单独添加20％时,可使GFPP阻燃等级达到UL–94 V0级;P–22单独添加20％,可使GFPP表面电阻率下降至1.4×108Ω.当阻...     

Synthesis of a novel,multifunctional inorganic curing agent and its effect on the flame‐retardant and mechanical properties of intrinsically flame retardant epoxy resin

Traditional curing agents have only a single property, while traditional synthetic organic flame‐retardant hardeners often show poor tolerance to oxidants, strongly acidic or alkaline reagents, and organic solvents and have toxicity problems. Here, a novel and multifunctional flame‐retardant curing agent of the inorganic substrate multifunctional curing agent of the inorganic substrate (FCIN) was proposed first and successfully prepared, and then an intrinsically flame‐retardant epoxy resin (EP) was prepared by covalently incorporating FCIN nanoparticles (FCINs) into the EP. The curing behavior of the FCINs was investigated, showing that FCIN/EP expresses a higher global activation energy than tetraethylenepentamine (TEPA)/EP and that the FCINs had strong interfacial adhesion to the EP matrix. Additionally, the FCINs were well dispersed and provided a remarkable improvement in mechanical and flame‐retardant properties of the intrinsically flame‐retardant EP. With the incorporation of 9 wt % FCINs into the EP, dramatic enhancements in the strength, modulus under bending, and toughness (～36%, ～109%, and ～586%, respectively) were observed, along with 85.2%, 46.4%, 98.3%, and 77.26% decreases in the peak heat release rate, total heat release, smoke production rate peak, and total smoke production, respectively, with respect to that of TEPA/EP. The mechanisms of its flame‐retardant, smoke‐suppression, and failure behaviors were investigated. The development of this unconventional, multifunctional flame‐retardant curing agent based on an inorganic substrate showed promise for enabling the preparation of a variety of new high‐performance materials (such as intrinsically flame‐retardant EP and functional modified polyesters). © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46410.