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1.
The present work aims to modify conventional epoxy resin by blending with four different phenolic–urea oligomers. These oligomers are similar to phenolic–urea resin matrix and simultaneously function as amino curing agent for epoxy matrix. In this context, phenolic–urea oligomers were prepared respectively by polycondensation reaction of four phenols namely phenol, m-cresol, resorcinol and 1,5-dihydroxy naphthalene, respectively with formaldehyde and urea in presence of acid catalyst. The resulting oligomers were characterized by elemental analysis, spectral studies (IR & NMR), number average molecular weight (M¯n) estimated by non-aqueous conductometric titration and thermal stability by thermogravimetric analysis (TGA). Each of these oligomers was used in resin matrix as a blending component for the modification of commercial epoxy resin for fabricating glass fiber reinforced laminates. Finally these laminates were evaluated for their synergetic thermal stability, mechanical properties and chemical resistance to different reagents.  相似文献   

2.
Hydroxyl‐terminated poly(ether ether ketone) with pendent tert‐butyl groups (PEEKTOH) was synthesized by the nucleophilic substitution reaction of 4,4′‐difluorobenzophenone with tert‐butyl hydroquinone with potassium carbonate as a catalyst and N‐methyl‐2‐pyrrolidone as a solvent. Diglycidyl ether of bisphenol A epoxy resin was toughened with PEEKTOHs having different molecular weights. The melt‐mixed binary blends were homogeneous and showed a single composition‐dependent glass‐transition temperature (Tg). Kelley–Bueche and Gordon–Taylor equations gave good correlation with the experimental Tg. Scanning electron microscopy studies of the cured blends revealed a two‐phase morphology. A sea‐island morphology in which the thermoplastic was dispersed in a continuous matrix of epoxy resin was observed. Phase separation occurred by a nucleation and growth mechanism. The dynamic mechanical spectrum of the blends gave two peaks corresponding to epoxy‐rich and thermoplastic‐rich phases. The Tg of the epoxy‐rich phase was lower than that of the unmodified epoxy resin, indicating the presence of dissolved PEEKTOH in the epoxy matrix. There was an increase in the tensile strength with the addition of PEEKTOH. The fracture toughness increased by 135% with the addition of high‐molecular‐weight PEEKTOH. The improvement in the fracture toughness was dependent on the molecular weight and concentration of the oligomers present in the blend. Fracture mechanisms such as crack path deflection, ductile tearing of the thermoplastic, and local plastic deformation of the matrix occurred in the blends. The thermal stability of the blends was not affected by blending with PEEKTOH. © 2005 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 44: 541–556, 2006  相似文献   

3.
The properties of diglycidyl ether of bisphenol-A epoxy resin toughened with poly(ether sulfone ether ketone) (PESEK) and poly(ether sulfone) (PES) polymers were investigated. PESEK was synthesised by the nucleophilic substitution reaction of 4,4’-difluorobenzophenone with dihydroxydiphenylsulfone using sulfolane as solvent and potassium carbonate as catalyst at 230 °C. The T g–composition behaviour of the homogeneous epoxy resin/PESEK blend was modelled using Fox, Gordon–Taylor and Kelley–Bueche equations. A single relaxation near the glass transition of epoxy resin was observed in all the blend systems. From dynamic mechanical analysis, the crosslink density of the blends was found to decrease with increase in the thermoplastic concentration. The storage modulus of the epoxy/PESEK blends was lower than that of neat resin, whilst it is higher for epoxy/PES blends up to glass transition temperature, thereafter it decreases. Scanning electron microscopic studies of the blends revealed a homogeneous morphology. The homogeneity of the blends was attributed to the similarity in chemical structure of the modifier and the cured epoxy network and due to the H-bonding interactions between the blend components. The fracture toughness of epoxy resin increased on blending with PESEK and PES. The increase in fracture toughness was due to the increase in ductility of the matrix. The thermal stability of the blends was comparable to that of neat epoxy resin.  相似文献   

4.
Organic–inorganic polymer hybrid films of epoxy polymer were prepared, using Cobaltous sulfate heptahydrate (CoSO4.7H2O) as a filler component, by physical blending method. UV–Vis optical absorption spectra were analyzed to determine optical band gaps (Eg) of the hybrid material. FTIR studies revealed the interaction of inorganic component with molecules of the polymer matrix. Glass transition temperature (Tg) and degradation temperature were determined by DSC. TG analysis showed the improvement in thermal stability of prepared hybrid films. XRD patterns revealed the amorphous nature of the pure epoxy polymer. Additional sharp peaks were seen for higher filler levels (FLs), indicating self formed nanostructures in the material, which was also evident from SEM analysis.  相似文献   

5.
Benzoxazines modified epoxy hybrid polymer matrices were developed using benzoxazines (CBDDM and BMPBDDM) and epoxy resins (DGEBA, SE and EP-HTPDMS) to make them suitable for high performance applications. The benzoxazine-epoxy hybrid polymer matrices were prepared via in-situ polymerization and were investigated for their thermal, thermo-mechanical, mechanical, electrical and morphological properties. Two types of skeletal modified benzoxazines namely 1,1-bis(3-methyl-4-hydroxyphenyl)cyclohexane benzoxazine (CBDDM) and bis(4-maleimidophenyl) benzoxazine (BMPBDDM) were synthesized by reacting paraformaldehyde and 4,4′-diaminodiphenylmethane with 1,1-bis (3-methyl-4-hydroxyphenyl)cyclohexane and N-(4-hydroxyphenyl)maleimide respectively. Epoxy resins viz., diglycidyl ether of bisphenol-A (DGEBA), silicon incorporated epoxy (SE) and siliconized epoxy resin (EP-HTPDMS) were modified with 5, 10 and 15 wt% of benzoxazines using 4,4′-diaminodiphenylmethane as a curing agent at appropriate conditions. The chemical reaction of benzoxazines with the epoxy resin was carried out thermally and the resulting product was analyzed by FT-IR spectra. The glass transition temperature, curing behavior, thermal stability, char yield and flame resistance of the hybrid polymers were analysed by means of DSC, TGA and DMA. Mechanical properties were studied as per ASTM standards. The benzoxazines modified epoxy resin systems exhibited lower values of dielectric constant and dielectric loss with an enhanced values of of arc resistance, glass transition temperatures, degradation temperatures, thermal stability, char yield, storage modulus, tensile strength, flexural strength and impact strength.  相似文献   

6.
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 (Tg) 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.  相似文献   

7.
The epoxy resins containing imine bonding were prepared from hydroxyl substituted Schiff base monomers in two steps. At the first step, hydroxyl substituted Schiff base monomers were synthesized via condensation reaction. At the second step, epoxy resins were synthesized from the reaction between Schiff base monomers and epichlorohydrine (EPC). Then curing processes of epoxy resins were achieved by p-phenylenediamine compound. The structures of resulting compounds were confirmed by FT-IR, UV-Vis and 1H-NMR. TG-DTA and DSC measurements were performed for thermal characterizations of the compounds. Chemical resistances of the cured epoxy-amine systems were determined for coating applications in acidic, alkaline and organic solvents. HCl (10%, aqueous solution), NaOH (10%, aqueous solution), DMSO, DMF, N-methylpyrrolidone, ethanol, THF and acetone were used for corrosion tests. Chemical resistance data of the synthesized epoxy resins demonstrated that they have good chemical resistance against various acid, alkaline and common organic solvents. Surface morphologies of epoxy resin and the cured epoxy resin were determined with scanning electron microscopy (SEM) measurements. Also, optical band gap (Eg) values of Schiff base monomers and epoxy resins were calculated from UV-Vis measurements.  相似文献   

8.
Polyureas having different heterocyclic groups were reacted, respectively, with commercial epoxy resins, i.e., diglicidyle ether of bisphenol A and brominated DGEBA. The resultant polyurea–epoxy systems were designated as I(a–f) and II(a–f), respectively. All the polyurea–epoxy systems were characterized by FTIR spectral studies, thermogravimetric analysis and number average molecular weight, estimated by non-aqueous conductometric titration. The polyurea–epoxy systems were then mixed with appropriate amounts of DGEBA epoxy resin, monitored for differential scanning calorimetry, and, based on this, glass fiber-reinforced composites were prepared. All the resultant laminates were characterized by physical and mechanical properties.  相似文献   

9.
Activated carbon derived from oil palm empty fruit bunch (AC-EFB), bamboo stem (AC-BS), and coconut shells (AC-CNS) were obtained by pyrolysis of agricultural wastes using two chemical reagents (H3PO4 or KOH). The AC-EFB, AC-BS and AC-CNS were used as filler in preparation of epoxy nanocomposites. Epoxy nanocomposites prepared at 1, 5 and 10 % activated carbons filler loading using KOH and H3PO4 chemical agents. Transmission electron microscopy confirms better dispersion of the nano-activated carbons in the epoxy matrix at 5 % activated carbon. The presence of 5 % AC-CNS in the epoxy matrix using H3PO4 chemical reagent resulted in an improvement of the thermal stability of epoxy matrix. KOH treated AC filled epoxy nanocomposites were slightly better in thermal stability as compared to H3PO4 treated AC filled epoxy nanocomposites, may be due to better interaction of filler with epoxy matrix. Thermal analysis results showed that thermal stability of the activated carbon filled epoxy nanocomposites improved as compared to the neat epoxy matrix. The degree of crystallinity of epoxy matrix was improved by adding the activated carbon due to interfacial interaction between AC and epoxy matrix rather than loading of AC alone. Developed nanocomposites from biomass (agricultural wastes) materials will help to reduce the overall cost of the materials for its demanding applications as insulating material.  相似文献   

10.
In an effort to combine and tailor the properties of thermoplastic resins we have investigated the synthesis of polyimide–polyformal block copolymers prepared by the condensation reaction of α,ω-diamino functionalized polyformal oligomers with α,ω-dianhydride terminated polyimide oligomers. Amino functionalized polyformal oligomers were synthesized by displacement condensation reactions of various bisphenols with methylene dihalides in the presence of base and aminophenols. Oligomeric aromatic polyformals having weight average molecular weights (MWw) of 7500 to 40,000 were obtained. Anhydride terminated polyimide oligomers with molecular weights (MWw) ranging from 10,000 to 15,000 were obtained by the condensation of bisphenol-A–dianhydride and aromatic amines. Combining the polyimide oligomers with the polyformal oligomers in dipolar aprotic or nonpolar solvents afforded the desired block copolymers. The polyimide–polyformal block copolymers generally display two distinct glass transition temperatures by differential scanning calorimetry. The (AB)n block copolymers were evaluated by TGA in both air and N2 for thermal/oxidative stability.  相似文献   

11.
Composites of a fumed silica industrial residue and an epoxy resin were prepared and their thermal stability and thermal degradation behaviour were studied by TGA in air. Classical thermal stability parameters, based on the initial decomposition temperature (IDT), temperature of maximum rate of mass loss (Tmax) and integral procedure decomposition temperature (IPDT) were calculated before and after subtraction of the filler mass from the TGA curves. Without filler mass subtraction, the thermal stability of the epoxy resin seems to be improved and the mass loss rate was reduced by the addition of fumed silica. Nevertheless, after subtraction of the filler mass, the thermal degradation behaviour of the resin was only slightly affected by the silica content. A possible negative effect of the silica content on the cure was also found.  相似文献   

12.
This research aims to develop superhydrophilic fiberglass/epoxy nanocomposite (FGEC) laminates with high mechanical, thermal, and impact properties. In order to achieve this goal, functionalized graphene (FGA) was used as a nanofiller material to improve the mechanical, impact, and thermal behaviors of FGEC, while the plasma treatment helped to form the oxidized polar functional groups (C9O groups and C–O groups) on the fabricated FGEC laminates, thus modifying their hydrophilic behavior. The experiments were started with production of FGEC laminates by mixing FGA (0.05-0.4 wt%) with epoxy resin in presence of Acetone (to obtain better dispersion), followed by preparation of FGEC laminates using vacuum-assisted resin transfer and curing processes. Afterwards, the surfaces of the fabricated FGEC laminates were treated by air plasma at 13Pa and 30W for different treatment times in the range 5–30 min. Mechanical and impact properties of the untreated and treated laminates were investigated according to ASTM-D7025 and ISO 6603-2 standards, respectively. Also, thermal behavior of the laminates was investigated using a thermogravimetric analysis, while a high resolution camera was used to record and calculate a contact angle of the untreated and treated laminates. SEM and Optical Microscope was used to observe dispersion of FGA, microstructure, impact mechanism, and surface morphology of the fabricated FGEC matrix. Meanwhile, XPS was used to evaluate changes in the surface structures of the untreated and treated samples. The results showed that 0.35 wt% of FGA and 15-min exposure to plasma treatment were enough to improve tensile strength and impact energy of the laminates by 18% and 70%, respectively, and to decrease the water contact angle from 67° to 14°.  相似文献   

13.
Montmorillonite (MMT) was modified with the acidified cocamidopropyl betaine (CAB) and the resulting organo‐montmorillonite (O‐MMT) was dispersed in an epoxy/methyl tetrahydrophthalic anhydride system to form epoxy nanocomposites. The intercalation and exfoliation behavior of the epoxy nanocomposites were examined by X‐ray diffraction and transmission electron microscopy. The curing behavior and thermal property were investigated by in situ Fourier transform infrared spectroscopy and DSC, respectively. The results showed that MMT could be highly intercalated by acidified CAB, and O‐MMT could be easily dispersed in epoxy resin to form intercalated/exfoliated epoxy nanocomposites. When the O‐MMT loading was lower than 8 phr (relative to 100 phr resin), exfoliated nanocomposites were achieved. The glass‐transition temperatures (Tg's) of the exfoliated nanocomposite were 20 °C higher than that of the neat resin. At higher O‐MMT loading, partial exfoliation was achieved, and those samples possessed moderately higher Tg's as compared with the neat resin. O‐MMT showed an obviously catalytic nature toward the curing of epoxy resin. The curing rate of the epoxy compound increased with O‐MMT loading. © 2004 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 42: 1192–1198, 2004  相似文献   

14.
Bisphenol A based low-molecular-weight epoxy resin was modified with epoxidized soybean oil, which exhibit viscosity reducing ability comparable to commercial grade active diluents. The studied compositions showed a non-Newtonian rheological behavior, typical for Bingham liquids. The values of the flow index (n) and the consistency index (k) for the compositions tested in the temperature range 25–65 °C were calculated from the Ostwald-de Waele rheological model and were used to calculate the flow-activation energy (Ea) using the Arhenius equation. Studies of co-crosslinking of mixed oil-resin compositions using isophorone diamine showed essential decrease of the reaction heat and peak maximum temperature. Mechanical properties, thermal stability, water absorption and chemical resistance of the epoxy resin modified with natural oil, were also investigated. Compositions of epoxy resin Ruetapox 0162, modified with the oil diluent, preserved very good mechanical properties of the epoxy resins and demonstrated relatively low water absorption as well as high chemical resistance. The compositions displayed even higher impact strength than pure epoxy resin due to plasticizing effect of the built-in oil. Compositions with the high contents (up to 60 weight %) of the oil were flexible materials with fast elastic recovery.  相似文献   

15.
A reactive amino-ended toughener was blended with different commercial epoxy resins namely, diglycidyl ether of bisphenol A, diglycidyl ether of bisphenol F, diglycidyl p-aminophenol and 1,5-naphthalenediamine as curing agent. The toughener was an aromatic amino-ended copolyethersulphone (coPES):poly(ether-sulphone)–poly(etherether-sulphone). The effect of the toughener on the thermal decomposition and char oxidation behaviour of the epoxy resins was studied by the simultaneous differential thermal analysis and thermogravimetric techniques. The glass transition temperature (T g) as well as characteristic parameters of decomposition, initial decomposition temperature (T i) and temperature at maximum degradation rate (T m), in both inert and oxidative environments, were determined in order to verify the influence of toughener on the thermal degradation of the different epoxy systems. It was observed that the presence of coPES maintains the high level thermal stability of the resin and that the glass transition temperature increase with the toughener percentage.  相似文献   

16.
Novel microcapsules (MCs) with organic/inorganic hybrid shell were successfully fabricated using epoxy resin as core material and nano boron nitride (BN) and mesoporous silica (SBA‐15) as inorganic shell materials in aqueous solution containing a water‐compatible epoxy resin curing agent. The morphologies, thermal properties and Young's moduli of MCs were investigated. The results indicated that epoxy resins were encapsulated by BN/SBA‐15/epoxy polymer hybrid layer, the resulting MCs were spherical in shape and the introduction of inorganic particles made MCs had rough surface morphology. The mean modulus value of MCs was from 2.8 to 3.1 GPa. The initial decomposition temperature (Tdi) of MCs at 5 wt% weight loss was from 309 to 312°C. MCs showed excellent thermal stability below 260°C. The structures and properties of MCs could be tailored by controlling the weight ratio of inorganic particle. When the weight ratio of BN to SBA‐15 was 0.15:0.10, MCs had the highest Tdi and modulus. The resulting MCs were applied to high performance 4,4′‐bismaleimidodiphenylmethane/O,O′‐diallylbisphenol A (BMI/DBA) system to design high performance BMI/DBA/MC systems. Appropriate content of MCs could improve the fracture toughness and maintain the glass transition temperature (Tg) of BMI/DBA system. The core materials released from fractured MCs could bond the fracture surfaces of the BMI/DBA matrix through the polymerization of epoxy resins. When the healing temperature schedule of 100°C/2h+150°C/1h was applied, 15 wt% MCs recovered 98% of the virgin fracture toughness of BMI/DBA. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

17.
Dynamic mechanical analysis was conducted on specimens prepared from cyanate ester (CE) and epoxy (EP) resins cured together at various mass compositions. Increase of amount of epoxy resin in composition was shown to have a disadvantageous effect on glass transition temperature (T g). It was shown that post-curing procedure was needed to produce a polymer matrix with a single glass transition relaxation, but increase in post-cure temperature up to 250 °C resulted in slight reduction in T g for epoxy/cyanate copolymers. TG results proved that the presence of epoxy resin reduces thermal stability of the cyanate/epoxy materials. The neat CE and EP/CE systems containing 30 wt% of epoxy resin were modified using epoxy-terminated butadiene–acrylonitrile rubber (ETBN) and polysiloxane core–shell elastomer (PS). The scanning electron microscopy (SEM) results showed the existence of second phase of ETBN and PS modifiers. Only in the case of EP/CE composition modified with ETBN, well-dispersed second phase domains were observed. Analysis of SEM images for other CE- and EP/CE-modified systems revealed the formation of spherical aggregates.  相似文献   

18.
New organic‐inorganic hybrid materials and their anti‐electrostatic hybrid membranes are prepared via sol‐gel process. The polycondensation of epoxy oligomers and AEAPS/Al2O3 complexes which are organically surface modified submicrometer aluminum trihydroxide inorganic fillers with an active aminoterminal silane coupling agent, N‐(2‐aminoethyl)‐3‐aminopropyltrimethoxysilane (AEAPS), are performed. AEAPS enhances the interfacial interactions between the inorganic fillers and epoxy polymers. Meanwhile, this coupling agent maintains well dispersion of fillers in these composites. To improve the mechanical strength and thermal stability, pyromellitic dianhydride (PMDA) is used as curing agent. These hybrid films prepared from this method have excellent physical properties, such as UV‐shielding, high transmission in visible resign (> 85%), high hardness (7~8H) , high adhesive force (7~8) and low relative surface resistance (9.71 × 1011~1.26 × 1010 Ω/cm2) with anti‐electrostatic characters. For thermal resistance, the best Td value of epoxy/PMDA/AEAPS/Al2O3 is 378.6 °C which is 85.4 °C higher than that of neat epoxy resin. Physical properties of these materials are almost the same as those of the nanocomposites prepared from expensive colloid Al2O3. Evidences from TEM micrograph show that the inorganic additives are dispersed evenly in organic matrix with nanometer scale.  相似文献   

19.
Nonaqueous synthesis of nanosilica in diglycidyl ether of bisphenol‐A epoxy (DGEBA) resin has been successfully achieved in this study by reacting tetraethoxysilane (TEOS) directly with DGEBA epoxy matrix, at 80 °C for 4 h under the catalysis of boron trifluoride monoethylamine (BF3MEA). BF3MEA was proved to be an effective catalyst for the formation of nanosilica in DGEBA epoxy under thermal heating process. FTIR and 29Si NMR spectra have been used to characterize the structures of nanosilica obtained from this direct thermal synthetic process. The morphology of the nanosilica synthesized in epoxy matrix has also been analyzed by TEM and SEM studies. The effects of both the concentration of BF3MEA catalyst and amount of TEOS on the diameters of nanosilica in the DGEBA epoxy resin have been discussed in this study. From the DSC analysis, it was found that the nanosilica containing epoxy exhibited the same curing profile as pure epoxy resin, during the curing reaction with 4,4′‐diaminodiphenysulfone (DDS). The thermal‐cured epoxy–nanosilica composites from 40% of TEOS exhibited high glass transition temperature of 221 °C, which was almost 50 °C higher than that of pure DGEBA–DDS–BF3MEA‐cured resin network. Almost 60 °C increase in thermal degradation temperature has been observed during the TGA of the DDS‐cured epoxy–nanosilica composites containing 40% of TEOS. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 757–768, 2006  相似文献   

20.
Composites based on conductive organic/inorganic fillers dispersed in insulating matrix have been widely investigated because of their widespread applications such as electromagnetic shielding, electrostatic discharge, and sensors. In this context, novel composite materials based on epoxy resin matrix charged with polyaniline (PANI)‐doped para‐toluene sulfonic acid were elaborated. Fourier transform infrared spectroscopy, X‐ray diffraction and scanning electron microscopy were used to check the structure and the morphology of the samples. Viscoelastic behavior and thermal stability of the composites were explored by dynamic mechanical thermal analysis and thermogravimetric analysis. It was shown that the PANI particles exhibited a partial crystalline structure and were homogeneously dispersed in epoxy matrix. Consequently, this structure affected the thermal stability and viscoelastic properties of the composites. Furthermore, the dielectric and electrical properties were investigated up to 1 MHz. Measurements of dielectric properties revealed that with loading fillers in matrix, the dielectric parameters increased to high values at low frequency then decreased at values around 40 and 32 of real and imaginary parts, respectively, at 1 MHz with 15% of PANI content. Copyright © 2011 John Wiley & Sons, Ltd.  相似文献   

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