首先,以全氟(2-甲基-3-氧杂己基)氟化物(六氟环氧丙烷二聚体)和N-(β-氨乙基)-γ-氨丙基三甲氧基硅烷(KH792)为原料制备一种氟化硅氧烷,用FTIR和1HNMR表征其结构.然后,将氟化硅氧烷与聚醚胺共同固化环氧树脂DGEBA(双酚A型二缩水甘油醚),测试了改性环氧树脂复合材料的性能.结果表明,与未改性环氧树脂相比,加入氟化硅氧烷使含氟量1%(以DGEBA质量计)改性环氧树脂复合材料的表面静态水接触角由72.0°增至103.2°,表面能由(42.08±2.17)mN/m降至(20.55±1.45)mN/m,40 d吸水率由1.75%降至1.38%,有效提高了材料的疏水性;介电常数由3.83降低至3.63;材料热分解5%温度由339℃升高至347℃;拉伸及弯曲力学性能分别提高了8.5%及7.7%.含氟量为1%时,改性环氧树脂复合材料的综合性能最佳,差式量热扫描和动态力学性能测试结果表明,少量改性剂可以促进环氧树脂的固化反应,提高固化度和交联密度;当氟化硅氧烷添加量增加时,材料内部发生显著的微相分离并导致性能逐渐下降.
Perfluoropolyether siloxane was synthesized by ester-amide exchange reaction from KH550 and perfluoropolyether methyl ester which was prepared by the reaction of perfluoropolyether acyl fluoride with anhydrous methanol, and its structure was characterized by infrared spectroscopy. A coating was sprayed and cured on the surface of steel plate with a fluorine solvent diluted solution of perfluoropolyether siloxane. The effects of mass fraction of perfluoropolyether siloxane, curing temperature, and curing time on water contact angle of the coating were discussed. The corrosion resistance of the perfluoropolyether siloxane coating in 3.5% CH3COOH, 5.0% NaOH, and 3.5% NaCl solutions, and its mechanical stability, thermal stability, and durability were examined. The results showed that the coating prepared on steel plate with 0.1% perfluoropolyether siloxane by curing at 150 °C for 30 min had a water contact angle of 113.6°. The steel plate coated with perfluoropolyether siloxane had good resistance to acid and salt as well as mechanical stability, thermal stability, and durability.
以双(3-氨基苯基)苯基氧化膦(BAPPO)和癸二酸为单体,通过膦酰化反应合成了含磷半芳香聚酰胺(PA10I),特性黏度为0.62dL/g.利用红外光谱、核磁共振表征了PA10I的结构;利用差示扫描量热法和热重法研究了PA10I热性能,结果表明PA10I的玻璃化转变温度为161℃,热分解温度为405℃.用热重法研究了PA10I在N2中的热降解动力学,用Kissinger和Flynn-Wall-Ozawa 2种方法求得PA10I的热降解活化能分别为175.7和177.9kJ/mol.用Coats-Red fern法证明了PA10I的热降解机理为F1降解机理.
Blends of polyamide (PA) 6 and phosphorous-containing hyperbranched polyamide (HBPA) were prepared by melt extrusion with PA6 as matrix and HBPA as modifier. The rheological behaviors,tensile and impact properties and flame resistance of the blends were investigated through capillary rheometer,mechanical properties tests,LOI test and TG analysis . The results show that with the content of HBPA increasing,the non-Newtonian index of the blend melt is close to 1 gradually and the melt tends to be converted to Newtonian fluids,the apparent viscosity decreases and it indicates that the processing property of the blend is improved,the viscous flow activation energy increases and it indicates that the temperature sensitivity of the blend is enhanced. Adding a small amount of HBPA can improve the mechanical properties of the blend,when the mass fraction of HBPA is 0.5%, the tensile strength is highest and increases from 62.6 MPa of pure PA6 to 72.4 MPa,when the mass fraction of HBPA is 1%,the elongation at break and notched impact strength is highest and increases from 228.3%of pure PA6 to 284.7%and from 19.8 kJ/m2 to 24.5 kJ/m2 respectively. The LOI test and TG analysis show that HBPA can improve the flame resistance of PA6 by promoting condensed phase charring,and when the mass fraction of HBPA is 1.5%,the value of LOI is highest and up to 28.4%.
A novel phosphorus-contained semi-aromatic polyamide was prepared from bis(3-aminophenyl)pheny phos-phine oxide(BAPPO)and hexanedioic acid by Yamazaki phosphorylation method. The main factors,such as reaction tem-perature,monomer concentration,solvent and reaction time were investigated. The inherent viscosity of the polymer was 0.47 dL/g. The structure of the polymer was characterized by FTIR and1H NMR. The results of DSC and TGA showed the polymer exhibited high glass transition temperature and good thermal stability(Tg=206,℃,T5%=388.1,℃). The limited oxygen index of the thin film sample was 43%,which indicated that the polymer has excellent flame retardancy.
以双(3-氨基苯基)苯基氧化膦、间苯二胺和间苯二甲酰氯为单体,采用低温溶液缩聚合法合成了含磷芳香族聚酰胺,共聚物的比浓对数粘度为1.44~2.41 dL/g.用红外光谱、核磁共振表征了聚合物的结构.利用差示扫描量热法、热失重分析研究了聚合物的热性能,结果表明,随含磷单体的增加,共聚物的Tg略有升高;含磷单体的引入提高了聚合物热稳定性.薄膜的拉伸实验结果表明共聚物具有良好的力学性能.LOI测试表明含磷单体的引入显著提高了聚合物的阻燃性.
Multi-walled carbon nanotubes(MWCNTs)were oxidized with mixed acid,and then were functionized with phosphorus-containing compound 2-(6-oxido-6,H-dibenzoxa phosphorin-6-yl)-1 ,4-dihydroxy phenylene(DOPO-HQ). The functionalized carbon nanotubes(MWCNTs-P)were used to modify epoxy resin. The effects of MWCNTs and MWCNTs-P on the mechanical properties and the flame retardancy of the epoxy resin were compared. The results showed that both MWCNTs and MWCNTs-P can improve the mechanical properties of the epoxy resin,while the modification effect of MWCNTs-P was better. When the MWCNTs-P content was 0.5%,the impact strength of the epoxy resin increased by 232%. SEM images showed that the addition of carbon nanotubes improved the toughness of the epoxy resin. The tests of tensile properties and bending performance of the composites indicated that the best content of MWCNTs-P was 1.0%. Limiting oxygen index(LOI)test revealed that MWCNTs-P can improve the flame retardancy of the epoxy resin,and when MWCNTs-P content was 0.5%,the LOI reached to 30.2%.