环氧磷酸活性阻燃剂的合成及对环氧树脂酸酐固化物性能的影响

通过将环氧树脂和磷酸直接反应,制得了与环氧树脂相容性较好的新型含磷活性阻燃剂——环氧磷酸。研究了其对环氧树脂酸酐固化物阻燃性以及其它各种性能的影响。实验结果表明：该阻燃剂对环氧树脂固化物有较好的阻燃作用,能明显提高树脂固化物的残炭量。适量添加环氧磷酸可大幅度提高固化物的韧性,并且对固化物的硬度以及热稳定性影响不大。     

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。     

2-羧乙基苯基次膦酸阻燃/固化环氧树脂

分别以2-羧乙基苯基次膦酸为添加型和反应型阻燃剂,研究了2-羧乙基苯基次膦酸对固化剂1618/环氧树脂固化体系产物热稳定性的影响和2-羧乙基苯基次膦酸对环氧树脂的阻燃/固化作用。结果表明:2-羧乙基苯基次膦酸对固化剂1618/环氧树脂固化体系热稳定性的提高没有明显作用;2-羧乙基苯基次膦酸对环氧树脂有较好的阻燃/固化作用,固化后可得到具有高透明度和良好热稳定性的环氧树脂,且阻燃等级可达到UL94-V0。     

高性能阻燃环氧灌封胶的制备

采用双酚A型环氧树脂CY5995为基体树脂,酸酐HY227为固化剂,聚磷酸铵(APP)/氢氧化铝(ATH)为复配阻燃剂,硅微粉为填料,脂环族环氧树脂S-186为改性剂制备了环氧灌封胶.通过示差扫描量热分析、热失重分析和氧指数、阻燃级别、弯曲和拉伸强度等测试研究了阻燃剂配比、填料以及脂环族环氧树脂用量等对灌封胶性能的影响...     

含磷阻燃环氧树脂体系研究进展

简要介绍了磷系阻燃剂作为一类新型无卤阻燃剂的特点和阻燃机理,重点综述了含磷阻燃环氧树脂体系的含磷固化剂、含磷环氧化合物及含磷环氧半固化物和添加磷型阻燃的进展,并通过热稳定性、成炭率和极限氧指数（LOI）等阻燃性能参数揭示了各类方法的阻燃效果,最后对含磷阻燃环氧树脂体系研究的未来进行了展望。     

磷氮阻燃剂的合成及其在环氧树脂中的应用

由亚磷酸、乙腈和苯膦酰二氯(PPDC)合成了一种添加型阻燃剂——苯膦酰二氨基双乙基四膦酸(PAEPA)。通过FTIR和ESI-MS对PAEPA的结构进行了表征。并将PAEPA混入环氧树脂(EP)中制备了阻燃环氧树脂,通过TGA、UL-94测试和LOI测试考察了用三乙烯四胺(TETA)固化的环氧树脂的阻燃性和热性能。结果表明,当w(P)=2.6%时,环氧热固性材料表现出优异的阻燃性能,并通过了UL94实验的V-0等级,LOI为29.8%。热重分析结果表明:800℃的残炭量为17.7%。SEM结果表明:EP/TETA体系中的PAEPA明显促进环氧树脂形成更致密、丰富的密封炭层,以提高燃烧过程中基体的阻燃性能。     

含氮酚醛树脂及其对环氧树脂的阻燃改性

简要介绍了环氧树脂的阻燃处理方法,详细说明了新型含氮阻燃剂的特点,合成了含氮酚醛树脂并将其用于对环氧树脂的改性,制得了电性能、阻燃性能均较好的环氧树脂。     

电子模块灌封用柔性阻燃型改性环氧树脂研究

选用柔性环氧树脂、活性增韧剂、磷系列阻燃剂FR-P和复合阻燃剂FR-A对环氧树脂CYD128进行改性,提高环氧树脂的柔韧和阻燃等性能,取得良好的改性效果,成功制备出柔性阻燃环氧电子灌封材料, 有利于解决环氧树脂在电子工程应用过程中的问题。     

四溴双酚A市场前景可观

四溴双酚A作为溴素阻燃剂中的一种,广泛用于合成材料的阻燃,以其毒性较低,与基材相溶性好而得到广泛的应用,作为添加剂主要应用于环氧树脂、ABS、HIPS、酚醛树脂、不饱和聚氨酯等材料的阻燃,作为反应型阻燃剂大量用于生产溴代环氧脂中间体、溴代聚碳酸酯,另外它还可用来合成更高档次的阻燃剂.……     

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。     

酚醛树脂基耐磨复合材料的改性及性能

采用原位改性法合成腰果酚改性酚醛树脂,并与粒径不同的碳化硅(SiC)混合物复配制备了腰果酚改性酚醛树脂基耐磨复合材料。通过红外光谱证明成功合成了腰果酚改性酚醛树脂,且树脂符合磨具磨料用液体树脂的基本要求。扫描电镜SEM图及力学性能测试结果表明,与普通酚醛树脂相比,腰果酚改性酚醛树脂粘结Si C的能力更强,且偶联剂的加入能提高树脂与碳化硅之间的相容性。在腰果酚含量为15%时,固化剂含量为10%,偶联剂含量为2.5%时,改性酚醛树脂基复合材料的拉伸、弯曲等力学性均能达到最优。通过分析耐磨测试结果发现,二硫化钼的添加能有效降低复合材料的磨损率,提高腰果酚改性酚醛树脂基耐磨复合材料的耐磨性。     

酚醛树脂砂在油井固砂中的应用研究

分别合成了热塑性和热固性酚醛树脂,将2者混合后加入固化剂并与砂混合得到酚醛树脂覆膜砂并测试了其拉伸强度、弯曲强度,渗透性和热老化性能。结果表明,当酚醛树脂质量占砂子总质量的3%时,覆膜砂力学强度和渗透性满足再造井壁要求。采用热固性酚醛树脂与六次亚甲基四胺协同固化热塑性酚醛树脂,产品强度高,储存稳定性好。     

Renewably sourced phenolic resins from lignin bio‐oil

Traditional lignin pyrolysis generates a bio‐oil with a complex mixture of alkyl‐functionalized guaiacol and syringol monomers that have limited utility to completely replace phenol in resins. In this work, formate assisted fast pyrolysis (FAsP) of lignin yielded a bio‐oil consisting of alkylated phenol compounds, due to deoxyhydrogenation, that was used to synthesize phenol/formaldehyde resins. A solvent extraction method was developed to concentrate the phenolics in the extract to yield a phenol rich monomer mixture. Phenolic resins were synthesized using phenol (phenol resin), FAsP bio‐oil (oil resin), and an extract mimic (mimic resin) that was prepared to resemble the extract after further purification. All three phenolic sources could synthesize novolac resins with reactive sites remaining for subsequent resin curing. Differential scanning calorimetry and thermogravimetric analysis of the three resins revealed similar thermal and decomposition behavior of phenol and the mimic resins, while the oil resin was less stable. Resins were cured with hexamethylenetetramine and the mimic resin demonstrated improved curing energies compared to the oil resin. The adhesive strength of the mimic resin was found to be superior to that of the oil resins. These results confirmed that extracting a mixture of substituted aromatics from FAsP bio‐oil could synthesize resins with properties similar to those from phenol and improved over the parent bio‐oil. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44827.     

Hybrid Polymer Networks of Epoxy Resin and Substituted Phenolic Novolacs

Hybrid polymer networks of diglycidyl ether of bisphenol (DGEBA) resin and phenolic novolac resins were prepared and tested for mechanical properties, hardness, and water absorption. The novolacs employed were based on each of phenol and substituted phenols such as p-cresol, t-butyl phenol, and cardanol. Cardanol is the main constituent of cashew nut shell liquid (CNSL), a renewable resource. Blends containing 10–15 wt% of novolac resin show substantial improvement in properties. These properties show a declining trend with higher novolac loading. The stoichiometric ratio between phenol and formaldehyde in the novolacs was optimized (1:0.8) for maximum property enhancement. The property profiles of the epoxy/novolac networks show that novolacs are effective modifiers for commercial epoxy resin. Incorporation of novolacs of substituted phenols results in relatively greater improvement in energy absorption during failure.     

New bisphenol novolac epoxy resins for marine primer steel coating applications

Bisphenol derived from reaction of phenol with benzaldehyde was prepared in the presence of sulfuric acid as catalyst. Bisphenol novolacs were synthesized in both melting and solution processes using p-formaldehyde and formalin solution in the presence of oxalic acid catalyst. ¹H NMR analysis shows a high methylene bridge contents using the novolacs synthesized in a melting process. The bisphenol novolac epoxy resin was prepared by reaction with epichlorohydrine in the presence of sodium hydroxide as a catalyst. The prepared novolac epoxy resins were cured with 1,2-amino ethyl piperazine (AEP) as a curing agent. The cured resins were evaluated as organic coating for steel. The mechanical properties of the cured epoxy resins were evaluated by measuring both impact resistance and hardness. The chemical resistances of the cured resins were evaluated through salt spray resistance, hot water immersion, solvent resistance, acid and alkali resistance measurements. The data indicate that the cured epoxy resins have excellent chemical resistances as organic coatings among other cured resins.     

Ortho-Substituted Ortho-Cresol Novolac Resins as an Epoxy Resin Curing Agent

A series of ortho-substituted ortho-cresol novolac resins were synthesized and used as curing agents for epoxy resins. The chemical structures of different ortho-substituted ortho-cresol novolac resins were investigated by many measurements, such as FT-IR, ¹H NMR, and ¹³C NMR. The results indicated that the ortho-cresol novolac resin with the needed proportion of ortho-substitution was synthesized through the adjustment of the reaction conditions. The studies on the curing kinetics of ortho-cresol novolac epoxy resin cured by different ortho-cresol novolac resins showed that the activation energy was reduced with an increase in the proportion of ortho-ortho methylene bridges.     

Novel phosphorilated flame retardant thermosets: epoxy-benzoxazine-novolac systems

Modified novolac resins with benzoxazine rings were prepared and cured with isobutyl bis(glycidylpropylether) phosphine oxide (IHPOGly) as crosslinking agent. Their curing behaviour using different epoxy/phenol molar ratios and with or without triphenylphosphine as catalyst was studied. Two different phenolic groups react with oxirane ring, those initially free and those generated after benzoxazine ring opening. In absence of catalyst, it is not possible to distinguish between them. However, for the catalyzed curing of the highest modification degree benzoxazine based novolac resin is possible to distinguish both reactions. The thermal, thermomechanical and flame retardant properties of the cured materials were measured. V-O materials were obtained when the resins were tested for ignition resistance with the UL-94 test.     

双酚A型含氮酚醛树脂的合成及应用研究

以双酚A、甲醛和三聚氰胺等为原料合成了含氮酚醛树脂,并对环氧树脂的阻燃改性,制得了电性能良好且阻燃性优异的阻燃环氧树脂。     

快固型钛酸酯杂化酚醛树脂的合成

通过钛酸四丁酯与热塑性酚醛树脂(Novolac树脂)的酯交换反应合成了一类快速固化型杂化酚醛树脂,可加入六亚甲基四胺进行固化。通过红外、核磁、凝胶时间和粘度等测试研究了树脂的分子结构和理化性能。结果表明:随着钛酸四丁酯用量增大,杂化酚醛树脂的分子质量明显增大,凝胶时间缩短,杂化酚醛树脂溶液的粘度增大,并基本呈线性关系。钛酸酯键有效改进了酚醛树脂的粘接性。固化速率的加快来源于改性树脂分子质量的增大和钛酸酯结构对于固化反应的催化作用;而杂化酚醛树脂粘接性的提高是由于酚醛树脂中的钛酸酯结构起到了偶联剂作用。     

Aging and Thermal Studies on Epoxy Resin Modified by Epoxidized Novolacs

Epoxy resins are thermosetting polymers widely used for polymer composites, adhesives, high performance coatings, potting and encapsulation, and numerous other applications. These resins have excellent mechanical and electrical properties, low cure shrinkage, and good adhesion to most substrates. This study is an attempt to improve the thermal and aging characteristics of epoxy resin by blending with other multifunctional epoxies such as EPN and ECN. Bis-phenol A epoxy resins containing 2.5 to 20 wt% of epoxy novolac were cured in the presence of a polyamide hardener and tested for thermal and mechanical properties, hardness, water absorption, etc. Blends containing 10 to 15 wt% of epoxy novolac show substantial improvement in properties such as tensile strength, elongation, and energy absorbed to break. The novolac derived from p-cresol was better than that based on phenol in enhancing the properties. TGA, DSC, and DMA were employed for studying the thermal properties of the modified resin. The study reveals that modification using epoxy phenol and p-cresol novolac resins (EPN and ECN, respectively) improves the aging characteristics of the epoxy resin in addition to overall improvement of the mechanical properties.