Studies on the curing behavior,thermal, and mechanical properties of epoxy resin-co-amine-functionalized lead phthalocyanine

A high performance copolymer was prepared by using epoxy (EP) resin as matrix and 3,10,17,24-tetra-aminoethoxy lead phthalocyanine (APbPc) as additive with dicyandiamide as curing agent. Fourier-transform infrared spectroscopy, dynamic mechanical analysis (DMA), differential scanning calorimetric analysis (DSC), and thermogravimetric analysis (TGA) were used to study the curing behavior, curing kinetics, dynamic mechanical properties, impact and tensile strength, and thermal stability of EP/APbPc blends. The experimental results show that APbPc, as a synergistic curing agent, can effectively reduce the curing temperature of epoxy resin. The curing kinetics of the copolymer was investigated by non-isothermal DSC to determine kinetic data and measurement of the activation energy. DMA, impact, and tensile strength tests proved that phthalocyanine can significantly improve the toughness and stiffness of epoxy resin. Highest values were seen on the 20 wt% loading of APbPc in the copolymers, energy storage modulus, and impact strength increased respectively 388.46 MPa and 3.6 kJ/m², T_g decreased 19.46°C. TGA curves indicated that the cured copolymers also exhibit excellent thermal properties.     

Novel amine terminated elastomeric oligomers and their effects on properties of epoxy resins as a toughener

The objective of this study was to investigate the effects of amine terminated elastomeric epoxy tougheners on the mechanical and thermal properties of diglycidyl ether of bisphenol A based epoxy resin. The amine terminated polycaprolactone (PCL) (1) and PCL‐PDMS‐PCL (2) based oligomers were synthesized and characterized by FTIR spectroscopy. The stoichiometrical amount of the reactive oligomers as toughener, reactive epoxy resin and the curing agent, 4,4′‐diaminodiphenyl sulfone (DDS) were mixed and degassed. The homogenous mixtures were cured at 120°C into the preheated molds. The mechanical and thermal characterizations of toughened epoxy resin system were evaluated. It has been shown that the mechanical and thermal properties of toughened epoxy system vary as a function of the chemical structure and the concentration of rective oligomers. Higher mechanical properties were obtained for epoxy resin toughened by PCL‐PDMS‐PCL (2) based oligomer. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

呋喃改性胺固化环氧树脂的耐强碱性研究

制备了一种新型的环氧树脂室温固化剂-呋喃改性胺,并用该固化剂固化E-51环氧树脂,研究了其浇铸体经108℃、25%的NaOH水溶液处理后,力学性能和电性能随碱煮时间的变化关系,并且采用扫描电镜表征了碱煮前后其复合材料拉伸断面形貌。结果表明,改性胺用量为24phr时,浇铸体的力学性能最优。碱煮150min以后,树脂固化物的力学性能变化比较小,拉伸强度、拉伸弹性模量和冲击强度的保留率分别为93.6%、87.1%和86.5%,绝缘性能有所下降,介电常数和介质损耗出现起伏性变化。     

仲氨基笼型倍半硅氧烷改性室温固化环氧树脂的研究

采用直接水解法合成了氨丙基笼型倍半硅氧烷(OapPOSS)。为了改善POSS与环氧树脂的相容性和分散性,在OapPOSS基础上制备了仲氨基笼型倍半硅氧烷(SaPOSS),并将其用于E-51/脂肪胺室温固化环氧树脂改性,研究了SaPOSS对环氧树脂力学性能、玻璃化转变温度、介电性能的影响。结果表明:SaPOSS能显著提高树脂的冲击性能和耐热性,降低介电常数和介电损耗。当SaPOSS加入量为3%时,环氧树脂的冲击强度从原来的20.5kJ/m2,提高到了29.7kJ/m2,玻璃化转变温度从113℃提高到117℃,扫描电镜的观测结果与力学性能的变化趋势相一致。当SaPOSS加入量为5%时,介电损耗从原来的0.035降到了0.024,介电常数也有大幅下降。     

Polyimide–polydimethylsiloxane copolymers for low‐dielectric‐constant and moisture‐resistance applications

Novel, randomly coupled, soluble, segmented polyimide–polydimethylsiloxane (PI–PDMS) copolymers were prepared from aminoalkyl‐terminated polydimethylsiloxane (At–PDMS), 4,4′‐oxydianiline diamine, pyromellitic dianhydride, and 4,4′‐diphenylmethane diisocyanate (MDI). When At–PDMS was introduced into the polyimide chain, the polyimide copolymers exhibited lower dielectric constants and better moisture resistance and mechanical properties. The reductions in the dielectric constant of the PI–PDMS copolymers could be attributed to the incorporation of polydimethylsiloxane (PDMS) into the polyimide chain and the nanopores in the film generated by carbon dioxide evolvement during the reaction. The lowest dielectric constant was 2.58 with 25 wt % PDMS and 5 wt % MDI. In addition, the water contact angles of the resultant copolymers increased from 51 to 109° when the contents of PDMS increased from 0 to 25 wt %. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Synthesis and Characterization of Cycloaromatic Polyamines to Cure Epoxy Resin for Industrial Applications

Cycloaromatic polyamines based on aniline, 4,4′-diaminodiphenylmethane and formaldehyde have been synthesized varying the molar ratio of aniline and formaldehyde keeping the amount of 4,4′-diaminodiphenylmethane constant via a single-step process, coded as PO1, PO2 and PO3. The resinous material of polyamines has been employed for curing studies of commercially available epoxy resinsw. The effect of time, temperature and the concentration of polyamines as curing agent have been studied. The epoxy specimens were further used for testing different dielectric properties such as resistivity, dielectric strength, dissipation factor and dielectric constant with an objective of their application as dielectric materials.     

Epoxy/nano‐silica composites: Curing kinetics,glass transition temperatures,dielectric, and thermal–mechanical performances

Nano‐silica particles were employed for enhancement of epoxy vacuum pressure impregnating (V.P.I.) resin. The influences of nano‐silica particles on the curing reaction, glass transition temperatures, dielectric behavior, and thermomechanical performances were investigated. The activation energy (E) for the epoxy curing reaction was calculated according to Kissinger, Ozawa, and Friedman‐Reich‐Lev methods. The glass transition temperatures were determined by means of differential scanning calorimetry, dynamic mechanical analysis, dc conduction, and ac dielectric loss analysis. Relationships between the glass transformation behaviors, the thermomechanical performances, and the dielectric behaviors were discussed. The influences of nano‐silica particles on the mechanical properties were also discussed in terms of non‐notched charpy impact strength and flexural strength. The morphologies were studied by means of SEM and TEM. The results indicated that nano‐silica particles could effectively increase both the toughness and strength of epoxy resin at low loadings (no more than 3 wt %) when nano‐silica particles could be well dispersed in epoxy matrix without any great aggregations. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

固化剂对环氧包封料性能的影响

研究了以甲基四氢苯酐和间苯二胺作固化剂时 ,环氧树脂包封料的固化放热现象 ,测定了不同固化剂体系的包封料力学性能、电性能、密度和吸水性。结果表明 ,间苯二胺的活性大于酸酐固化剂的活性 ,但填料的加入使胺固化的放热降低 ,酸酐固化的升高。胺固化的冲击强度较高 ,加入填料可提高拉伸强度。胺固化的介电常数 ,介电损耗角较高 ,但体积电阻率较低 ,其吸水性较高     

Glass Fiber Reinforced Composites and Thermal Study of Flame Retardant Epoxy Resin Systems Using Anhydride Curing Agents

Differential scanning calorimetric (DSC) curing kinetics of the epoxy systems composed of conventional, tetrafunctional, and phosphorylated epoxy resins were investigated using different anhydrides as curing agents and triethylamine as curing catalyst. The dynamic scans were analyzed to estimate the activation energy and the order of reaction for the curing process using some empirical relations. The thermal stability of the cured epoxy resins was studied by thermogravimetric analysis in nitrogen atmosphere at a heating rate of 10°C/min. Glass fiber reinforced composites were fabricated and evaluated for their limiting oxygen index, mechanical properties, dielectric properties, and chemical resistance. The incorporation of an epoxy fortifier showed significant improvement in mechanical properties.     

酸酐固化聚二甲基硅氧烷改性环氧树脂体系的研究

合成了聚二甲基硅氧烷与环氧树脂的增容剂，以甲基四氢苯酐为固化剂固化聚二甲基硅氧烷改性环氧树脂体系，通过测定，中击强度、拉伸强度、弯曲强度分析了其增韧增强效果。结果表明，增容剂的加入提高了环氧树脂与聚二甲基硅氧烷的相容性，当聚二甲基硅氧烷的含量为10％时，改性环氧树脂体系的力学性能最好；并通过热失重法、差示扫描量热法测定了固化物的热性能，其耐热稳定性与纯环氧树脂相比有明显提高。     

Mechanical and dielectric properties of epoxy resin modified using reactive liquid rubber (HTPB)

In the present study, hydroxyl‐terminated polybutadiene (HTPB) liquid rubber was employed to modify epoxy resin using 2,4,6‐tri (dimethylaminomethyl) phenol as a catalyst, and methyl hexahydrophthalic anhydride as a curing agent. The reactions between HTPB and epoxy were monitored by Fourier transform infrared (FTIR); the mechanical and dielectric properties of HTPB modified epoxies were evaluated and the morphology was investigated through scanning electronic microscopy (SEM). The FTIR analysis evidenced the occurrence of a chemical reaction between the two components. The mechanical results indicated that the impact strength of HTPB‐modified epoxy was superior to that of the pure epoxy. As the HTPB content increased up to 10 phr the best mechanical performances in terms of tensile and flexural properties were achieved when compared to the unmodified epoxy. Higher concentration of HTPB resulted in larger particles and gave lower mechanical strength values. The incorporation of HTPB into epoxy decreased the dielectric constant and dissipation factor over a wide frequency range from 1 to 10⁶ Hz, and improved the electrical resistivity. SEM micrographs showed that the modified epoxy exhibited a two‐phase morphology where the spherical rubber domains were dispersed in the epoxy matrix. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

环氧树脂/石英纤维透波复合材料制备

为改善环氧树脂的介电性能及提升石英纤维的界面性能,使用缩水甘油醚基笼型倍半硅氧烷(G-POSS)和γ-氨丙基三乙氧基硅烷(KH-550)分别对环氧树脂和石英纤维进行改性.利用差示扫描量热法研究改性后环氧树脂的固化过程,并通过外推法确定了其固化工艺,根据固化工艺制备环氧树脂/石英纤维复合材料,分别对该复合材料的热稳定性、...     

Carbon fiber cardanol-epoxy composites

Carbon fiber composites based on tetrafunctional epoxy resin N,N,N′,N′-tetraglycidyl-2,2-bis[4-(4-aminophenoxy)phenyl]propane modified with cardanol were investigated. The differential scanning calorimetric technique was used to study the curing reaction of the neat resins. The dielectric properties of the composites were compared. The use of cardanol in epoxy resins at cardanol/epoxy molar ratios less than 0.3/1 improved the chemical resistance as well as the mechanical properties of the composites, such as the flexural strength and modulus, tensile strength and modulus, and interlaminar shear strength. Higher cardanol contents decreased such properties. The highest properties of the composites were observed with the epoxy-cardanol resin having a cardanol/epoxy molar ratio of 0.3/1. © 1996 John Wiley & Sons, Inc.     

微波技术在环氧树脂及其复合材料中的应用

论述了近年来微波固化技术在环氧树脂及其复合材料固化中的应用,重点比较了微波固化与传统热固化后环氧树脂及其复合材料的力学性能、热性能和粘结强度的变化,并对环氧树脂复合材料微波固化的研究进行了展望。     

环氧树脂聚酰胺网络体系性能研究

用红外光谱法表征了4种聚酰胺固化剂与环氧树脂按等当量配比,在一定条件下的固化反应过程。DSC法测定了其固化反应活性。桐马聚酰胺/环氧树脂固化体系较聚酰胺650/环氧树脂固化体系的固化活性大大提高,同时测定了该固化产物的热失重(TG)及玻璃化温度(Tg),对该固化物的热稳定性进行了评价,还测定了不同固化时间的剪切强度以研究其动态力学性能,从浇铸体的冲击强度方面比较其韧性。综合比较分析了聚酰胺固化剂与环氧树脂固化体系的力学性能、耐热性、电绝缘性等。结果表明:桐马聚酰胺Ⅲ型固化剂具有黏度低、粘接强度大、耐热性好、力学性能优等优点。     

Epoxidized pine oil‐siloxane: Crosslinking kinetic study and thermomechanical properties

In this study, a novel approach to toughen biobased epoxy polymer with different types of siloxanes was explored. Three different modified siloxanes, e.g., amine‐terminated polydimethyl siloxane (PDMS‐amine), glycidyl‐terminated polydimethyl siloxane (PDMS‐glycidyl), and glycidyl‐terminated polyhedral oligomeric silsesquioxane (POSS‐glycidyl) were used as toughening agents. The curing and kinetics of bioepoxy was investigated by differential scanning calorimetry and Fourier transform infrared spectroscopy. The mechanical, thermal, and morphological properties of the cured materials were investigated. Rheological characterization revealed that the inclusion of POSS‐glycidyl slightly increased the complex viscosity compared to the neat resin. The morphology of the cured bioresin was characterized by transmission electron microscopy and scanning electron microscopy. The inclusion of POSS‐glycidyl to bioepoxy resin resulted in a good homogeneity within the blends. The inclusion of PDMS‐amine or PDMS‐glycidyl was shown to have no effect on tensile and flexural properties of the bioresins, but led to a deterioration in the impact strength. However, the inclusion of POSS‐glycidyl enhanced the impact strength and elongation at break of the bioresins. Dynamic mechanical analysis showed that the siloxane modified epoxy decreased the storage modulus of the bioresins. The thermal properties, such as decomposition temperature, coefficient of linear thermal expansion, and heat deflection temperature were improved by inclusion of POSS‐glycidyl. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42451.     

Copolymers of phenolphthalein-aniline-based benzoxazine and biphenyl epoxy: curing behavior and thermal and mechanical properties

In this work, the crosslink density and mechanical properties of phenolphthalein-aniline-based benzoxazine (BP-a) were enhanced through blending with biphenyl epoxy. The curing behavior of the blends was explored, and the thermal and mechanical properties of the corresponding copolymers were investigated in detail. The results showed that these copolymers possessed higher initial decomposition temperatures and better mechanical properties but slightly lower glass transition temperatures and coefficients of thermal expansion than those of BP-a.     

Physical properties and shrinkage of epoxy resins cured with lactams

In order to reduce the shrinkage of epoxy resin during the curing process, lactam is incorporated into epoxy in a copolymerization reaction. In this study, various amounts of lactams and BF₃-MEA were added to epoxy, and the volume shrinkage of polymerization was investigated. It was found that shrinkage decreases with the increase of the lactam content and with the lactam ring size as well. Infrared spectroscopic analysis, scanning electronic microscopic analysis, and mechanical tests were used to investigate the structure and properties of the copolymers. The results show that the incorporation of caprolactam leads to an increase in tensile strength and elongation, but the Izod impact strength is not improved.     

Effect of polythiourethane hardener modification on the behaviour of epoxy resin

Polythiourethanes based on oligomeric polymercaptans were employed as curing agent of epoxy resin. The epoxy matrices, in the form of castings, were characterized for their mechanical properties such as tensile strength, elongation at break and unnotched Charpy impact strength as per ISO methods. Mechanical studies indicated that the incorporation of polythiourethane into epoxy resin improves the toughness and flexibility with reduction in tensile strength for samples cured at ambient conditions and influences the mechanical and thermal properties according to its percentage content for samples cured at 130°C. The high increase of impact strength was explained by the development of two-phase morphology during the cure process. The results of this study indicate that both the stoichiometry of the curing mixture and the initial thermal condition are of critical importance in governing the curing mechanism, structure of the network, morphology and the final properties of epoxy/polythiourethane compositions.     

Exploring the influence of co‐monomer content in the dry crosslinked ethylene octene copolymer based blends

This article illustrates the influence of co‐monomer content in the ethylene octene copolymer (EOC) on the dry curing process of EOC:PDMS rubber blends. The EOC:PDMS blends were prepared by melt mixing in an internal mixer and crosslinked through electron beam radiation method. During electron beam irradiation both the EOC and PDMS phase gets crosslinked; which is evident from the gel content study. From the rheology analysis, it is understood that the EOC with high octene (co‐monomer) content has better radiation crosslinkability as compared with the EOC with low co‐monomer content. Through radiation crosslinking, the physico‐mechanical properties of the EOC:PDMS system was improved significantly. The tensile strength of high co‐monomer content EOC:PDMS 70:30 blends were drastically improved by 49.5% on irradiation with a dosage of 75 kGy. Morphology study of the EOC:PDMS system were carried out by scanning electron microscopy (SEM) and correlated with the physico‐mechanical properties. The radiation crosslinked blends shows higher volume resistivity, lower dielectric constant, and loss as compared with the uncrosslinked counterparts. POLYM. ENG. SCI., 57:1016–1027, 2017. © 2016 Society of Plastics Engineers