Study of epoxy resin for cryogenic use by positron annihilation method

The molecular state of epoxy resins for cryogenic use has been studied in terms of positron lifetime measurement. The addition of plasticizer increased the free volume in the epoxy and hence the ductility of the epoxy at room temperature was increased. The fracture toughness at cryogenic temperatures, however, decreased. The increase of molecular weight between crosslinks decreased the free volume in the epoxy at room temperature and increased the fracture toughness slightly at cryogenic temperature. Based on the data the molecular state model desired for cryogenic application was proposed and the nano-sized silica dispersed epoxy was prepared by means of sol-gel method to follow the model. The cryogenic properties of the silica dispersed epoxy and the free volume evaluated by positron annihilation lifetime were also discussed.     

MODIFICATION OF EPOXY RESIN WITH POLYSILOXANE BEARING PENDANT QUATERNARY AMMONIUM GROUPS

Polysiloxane bearing pendant quaternary ammonium groups (PSI) was used to modify the surface properties ofepoxy resins. In the cured resin, PSI formed the dispersed phase. Remarkable enrichment and gradient distribution ofpolysiloxane on the surface region of the epoxy resins were demonstrated by XPS analysis. The composition and propertiesof the surface of PSI-modified epoxy resin, which is in contact with the mold, are dependent on the material of the mold.Through the incorporation of PSI, epoxy resins with low surface energy and low friction coefficient were obtained.Polysiloxane with lower ionic group content shows a higher degree of enrichment on the resin surface and leads to a highercontact angle against water, while the polysiloxane having optimum compatibility with the epoxy resin shows a greater effectin reducing the static friction coefficient of the resin against glass.     

Fracture toughness and surface morphology of micro/nano sized fibrils-modified epoxy resin

Two kinds of micro/nano sized fibrils based on cellulose (MFC) and polyvinyl alcohol (PVA) were used as reinforcer for epoxy resin (EP) with different contents in the range from 0 to 0.3 wt %. PVA nanofibers with diameter about 40–80 nm were fabricated by electrospinning technique. The analysis of mechanical properties showed that by both adding MFC and PVA to EP the fracture toughness was increased. The SEM results showed that micro/nano sized fibers dispersed throughout epoxy resin, prevented and changed the path of crack growth.     

Reactive Core-Shell Bottlebrush Copolymer as Highly Effective Additive for Epoxy Toughening

Herein,we designed a core-shell structured bottlebrush copolymer (BBP),which is composed of rubbery poly(butyl acrylate) (PBA)core and an epoxy miscible/reactive poly(glycidyl methacrylate) (PGMA) shell,as an epoxy toughening agent.The PGMA shell allows BBP to be uniformly dispersed within the epoxy matrix and to react with the epoxy groups,while the rubbery PBA block simultaneously induced nanocavitation effect,leading to improvement of mechanical properties of the epoxy resin.The mechanical properties were measured by the adhesion performance test,and the tensile and fracture test using universal testing machine.When BBP additives were added to the epoxy resin,a significant improvement in the adhesion strength (2-fold increase) and fracture toughness (2-fold increase in Klc and 5-fold increase in Glc)compared to the neat epoxy was observed.In contrast,linear additives exhibited a decrease in adhesion strength and no improvement of fracture toughness over the neat epoxy.Such a difference in mechanical performance was investigated by comparing the morphologies and fracture surfaces of the epoxy resins containing linear and BBP additives,confirming that the nanocavitation effect and void formation play a key role in strengthening the BBP-modified epoxy resins.     

Oligo-fluoropolymer Modified Cycloaliphatic Epoxy Resins with Excellent Compatibility,Waterproof and Mechanical Properties for LED Encapsulation

An oligo-fluoropolymer(PFM) with functional cycloaliphatic epoxy and fluorinated groups was obtained via free radical polymerization and applied to the modification of cycloaliphatic epoxy resins(CE). The chemical structure of PFM was characterized by Fourier transform infrared(FTIR) spectroscopy, gel permeation chromatography(GPC) and nuclear magnetic resonance(NMR) spectroscopy, and the effects of different PFM concentrations(0.5%—6%, mass fraction) on the thermal resistance, mechanical properties, surface dewettability, light transmission, refractive index and various cured polymer properties were studied in detail. The DSC and TGA results demonstrate that the modified epoxy resins possess a higher thermal resistance than the neat epoxy resin. The improvements in the surface dewettability and water resistance are caused by the high crosslinking density and the enrichment of the oligo-fluorinated random copolymers dispersed in the matrix. The fracture surface morphologies of the thermosets were investigated by scanning electron microscopy(SEM) and transmission electron microscopy(TEM). It was observed that the optical transmittance of the composites was maintained even though microphase separation occurred during the curing process. With respect to the corresponding properties of the neat epoxy resins, the 2 phr(parts per hundreds of resin) PFM thermoset exhibited relatively better comprehensive properties, making the cured material a good candidate for light-emitting diode(LED) encapsulation.     

增容剂对“壳－核”型共聚物增韧尼龙6的亚微形态与性能的影响

增容剂对“壳－核”型共聚物增韧尼龙６的亚微形态与性能的影响汪晓东，金东吉，金日光（北京化工大学６１信箱北京１０００２９）关键词尼龙６，“壳－核”型共聚物，增容剂，增韧，亚微相态采用乳液“壳一核”型共聚物增韧各种工程塑料近年来引起广泛的关注ｌ‘，’１．...     

Preparation and Characterization of Cyclohexyl Moiety Toughened POSS-Reinforced Epoxy Nanocomposites

Polyhedral oligomeric silsesquioxane (POSS)-reinforced epoxy nanocomposites were prepared by reacting commercially available diglycidyl ether of bisphenol-A (DGEBA) and tetraglycidyl diamino diphenyl methane (TGDDM) epoxy resins with 1,1-bis(3-methyl-4-glycidyloxyphenyl)cyclohexane (Cy-Ep) separately and reinforced with POSS nanocluster. POSS (OAPS)-reinforced hybrid Cy-Ep-epoxy resin castings were characterized for their mechanical and morphological properties. The data obtained from mechanical studies indicated that the incorporation of nano OAPS into Cy-Ep modified hybrid systems results in improved stability. Among the epoxy systems studied, the TGDDM-based hybrid epoxy system exhibited higher values of tensile and flexural properties than that of the DGEBA hybrid epoxy system, whereas the impact strength of the DGEBA system was higher than that of the TGDDM system. The dispersion of POSS was confirmed by scanning electron microscopy and visual observation studies.     

增容剂对“壳－核”型共聚物增韧尼龙6的亚微形态与性能的影响

增容剂对“壳－核”型共聚物增韧尼龙６的亚微形态与性能的影响汪晓东，金东吉，金日光（北京化工大学６１信箱北京１０００２９）关键词尼龙６，“壳－核”型共聚物，增容剂，增韧，亚微相态采用乳液“壳一核”型共聚物增韧各种工程塑料近年来引起广泛的关注ｌ‘，’１．...     

在Bu_2SnO-Bu_3PO_4缩合物的存在下以端羟基聚醚增韧环氧树脂

工业中大量生产的端羟基聚醚 ,由于羟基的反应活性不够 ,不能直接用于增韧胺类固化的环氧树脂 .Bu2 SnO Bu3PO4 缩合物能催化羟基对环氧基的加成反应 .本文研究在Bu2 SnO Bu3PO4 缩合物Sn P6 70 0的存在下以端羟基聚四氢呋喃 (PTMG)增韧芳香胺 4,4′ 二氨基二苯砜 (DDS)固化的环氧树脂 .PTMG首先与环氧树脂反应生成嵌段共聚物 ,在固化时发生微相分离 .分散相的尺寸在有利于增韧的范围内 .PTMG在分子量与浓度适当时 ,能使树脂的断裂韧性大大提高 ;抗弯强度也有显著提高 ,而Tg 和模量略有降低 .     

不完全相反转乳化过程分散相水滴形态发展研究

相反转乳化技术是制备高分子树脂水基分散体系的新方法[1～4].相反转指多组分体系(如油/水/乳化剂)中的连续相在一定条件下相互转化的过程,如在油/水/乳化剂体系中,其连续相由水相向油相(或从油相变为水相)的转变.在连续相转变区,体系的界面张力最低,因而分散相的尺寸最小.同理,可利用相反转技术直接将高分子树脂乳化为尺寸很小的水基微粒,即制备高分子树脂的水基分散体系.由于高分子树脂的粘弹性及相反转过程的复杂性,对高分子树脂的相反转乳化过程的机理研究较少.杨振忠[5]等通过调节高分子非离子型乳化剂浓度,可以有效地控制相反转完善程…     

具高耐热性多芳烃结构环氧树脂的研究

综述了近年来具耐热性多芳烃结构环氧树脂的发展概况,包括萘系、蒽系和芘系环氧树脂,着重介绍了其合成途径、反应活性及结构与性能的关系.认为多芳烃结构环氧树脂具有良好的耐热耐湿性,颇具发展潜力.其中,萘系环氧树脂与蒽、芘系环氧树脂相比 ,具有较高的反应活性和耐热性,具有较高的实际应用价值.因此,近年来萘基环氧树脂受到研究人员和厂商的关注,并且一些萘系环氧树脂已经应用于生产.     

化学结构变化对刚棒状环氧树脂相行为和热力学性能的影响

用线性酚醛树脂(PN)和4-氨基苯基氨基砜(SAA)作为固化剂, 与刚性棒状环氧树脂联苯环氧(DGEBP)、四甲基联苯环氧(DGETMBP)和传统双酚A环氧树脂(DGEBA)分别进行固化. 研究了固化剂和环氧树脂化学结构的改变对热固网络相行为和热力学性能的影响. 结果表明, 刚性环氧网络比传统的DGEBA具有更好的热力学性能. DGEBP可形成不同类型的取向网络, 而取向态的类型也直接影响了热固网络的热力学性能. 用扫描电镜(SEM)观察不同网络体系的断裂面结构, 发现取向的刚性棒状环氧网络的断裂面呈韧性断裂, 而其它无定形环氧网络则呈典型的脆性断裂.     

磷系阻燃环氧树脂研究

本文对近年来国内外9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物（DOPO）衍生物的合成及其应用于阻燃环氧树脂的方法进行介绍,并对所显示的阻燃性、热性能等作了概述和比较。将反应型磷系阻燃剂DOPO衍生物引入环氧树脂基体结构中形成阻燃持久、无卤、低烟、无毒、热稳定性好的新型含磷环氧树脂。     

Preparation and properties of epoxy resins cured with silyl esters of phenol novolak and cresol novolak

The curing agents of epoxy resin, trimethylsilyl ethers of phenol novolak (TMSPN) and cresol novolak (TMSCN) were prepared by refluxing phenol novolak and cresol novolak respectively, with the mixture of hexamethyldisilazane and chlorotrimethylsilane in THF. The curing reaction of epoxy resin with these curing agents and the thermal properties of cured resins were examined. The Tg values of epoxy resins cured with TMSPN were a little higher than those cured with TMSCN. The maximum of Tg is 118°C for TMSPN-cured epoxy resin against 112°C for TMSPN-cured epoxy resin. The water absorption of hydrophobic epoxy resins cured with TMSPN was a little lower than those cured with TMSCN. The clear decrease of water absorption is attributed to the difficulty of the micro-void formation caused by the more tight primary structures of TMSPN. The water absorption at 25°C containing trimethylsilyl groups is about one-tenth of that of epoxy resins cured with conventional curing agents and even one-half of that of the epoxy resins cured with active esters. The low water absorption is attributed to the presence of trimethylsilyl groups, which are more hydrophobic than ester groups, and to the absence of hydroxyl groups of the cured resins. This revised version was published online in July 2006 with corrections to the Cover Date.     

PHASE STRUCTURE AND PROPERTIES OF EPOXY RESIN MODIFIED BY POLYSILOXANE BEARING PENDANT AMINO GROUPS

Polysiloxane-modified epoxy resins were prepared through the reaction of epoxy resin with polydimethylsiloxanesbearing pendant N-(β-aminoethyl)-γ-aminopropyl groups. The morphology and properties of the cured epoxy resins modifiedby the polysiloxanes were investigated. It was found that the phase structure and properties of the cured epoxy resins dependmainly on the amino group content in the polydimethylsiloxane and the level of the modifier. The change of phase structurein the cured epoxy resin systems was responsible for the dramatic change in their mechanical and surface properties.     

咪唑固化不同类型环氧树脂的固化特征、固化动力学及其反应活性

以咪唑为固化剂,对缩水甘油醚型、缩水甘油酯型环氧树脂(简称链型环氧树脂)及脂环环氧树脂的固化特征、固化动力学及反应活性进行了研究.DSC实验结果表明,固化过程均分两阶段进行,链型环氧树脂固化反应表观活化能低于脂环环氧树脂.各树脂第一阶段的表观反应活化能均低于第二阶段活化能.当脂环环氧树脂中混入不同比例的链型环氧树脂后,固化反应速率均较脂环环氧树脂单独固化时快,当链型环氧树脂量大于50％时,更为明显.     

Synthesis and thermal characterization of phosphorus containing siliconized epoxy resins

Siliconized epoxy matrix resin was developed by reacting diglycidyl ethers of bisphenol A (DGEBA) type epoxy resin with hydroxyl terminated polydimethylsiloxane (silicone) modifier, using γ-aminopropyltriethoxysilane crosslinker and dibutyltindilaurate catalyst. The siliconized epoxy resin was cured with 4, 4-diaminodiphenylmethane (DDM), 1,6-hexanediamine (HDA), and bis (4-aminophenyl) phenylphosphate (BAPP). The BAPP cured epoxy and siliconized epoxy resins exhibit better flame-retardant behaviour than DDM and HDA cured resins. The thermal stability and flame-retardant property of the cured epoxy resins were studied by thermal gravimetric analysis (TGA) and limiting oxygen index (LOI). The glass transition temperatures (T_g) were measured by differential scanning calorimetry (DSC) and the surface morphology was studied by scanning electron microscopy (SEM). The heat deflection temperature (HDT) and moisture absorption studies were carried out as per standard testing procedure. The thermal stability and flame-retardant properties of the cured epoxy resins were improved by the incorporation of both silicone and phosphorus moieties. The synergistic effect of silicone and phosphorus enhanced the limiting oxygen index values, which was observed for siliconized epoxy resins cured with phosphorus containing diamine compound.     

活性酯固化环氧树脂物性的研究

主要对活性酯固化环氧树脂的吸水性、高耐湿性、电气特性等方面进行了研究,同时也对其树脂极性、交联结构、分子链运动等方面也进行了研究．     

Flame-retardant epoxy resins based on phthalide derivative

The phthalide-containing epoxy resins are synthesized and characterized in comparison with the bisphenol-A epoxy resins in terms of thermal properties. Although both resins contain comparable amounts of halogens, the resulting flame retardancy is higher in the phthalide-containing resin. The char formation upon pyrolysis is also enhanced by the phthalide functionality.     

Synthesis and properties of novel fluorinated epoxy resins based on 1,1-bis(4-glycidylesterphenyl)-1-(3′-trifluoromethylphenyl)-2,2,2-trifluoroethane

A novel fluorinated epoxy resin, 1,1-bis(4-glycidylesterphenyl)-1-(3′-trifluoromethylphenyl)-2,2,2-trifluoroethane (BGTF), was synthesized through a four-step procedure, which was then cured with hexahydro-4-methylphthalic anhydride (HMPA) and 4,4′-diaminodiphenyl-methane (DDM). As comparison, a commercial available epoxy resin, bisphenol A diglycidyl ether (BADGE), cured with the same curing agents was also investigated. We found that the BGTF gave the exothermic starting temperature lower than BADGE no mater what kind of curing agents applied, implying the reactivity of the former is higher than the latter. The fully cured fluorinated BGTF epoxy resins have good thermal stability with glass transition temperature of 170-175 °C and thermal decomposition temperature at 5% weight loss of 370-382 °C in nitrogen. The fluorinated BGTF epoxy resins also showed the mechanical properties as good as the commercial BADGE epoxy resins. The cured BGTF epoxy resins exhibited improved dielectric properties as compared with the BADGE epoxy resins with the dielectric constants and the dissipation factors lower than 3.3 and dissipation 2.8 × 10⁻³, respectively, which is related to the low polarizability of the C-F bond and the large free volume of CF₃ groups in the polymer. The BGTF epoxy resins also gave low water absorption because of the existence of hydrophobic fluorine atom.