| PMIA, as a very important high-performance polymer materials, with high heat resistance performance and spinning capability is much better than other polymer materials, and as a high-temperature flame-retardant fiber it has been developed rapidly. But polyarylamide stability in post-combustion carbon layer is not good enough, In recent years, in the main chain, introduced by copolymerization retardant elements and groups, preparation of flame-retardant fibers are getting more and more attention, because the flame-retardant performance effect lasting, non-volatile, non-migratory, environmentally friendly, conducive spun fiber, so it represents a development direction of retardant fibrous material. Therefore, the design and synthesis of inter-aramid modified is further improved the flame resistance, oxidation stability, increase the amount of char, so there is a theoretical value and practical significance for this thesis.Firstly, in this thesis, we created thesynthesis of monomer BNPPO, Under the optimal reaction conditions in 78% yield through BNPPO and N-bromosuccinimide (NBS) we have the solvent reaction of monomers synthesized bis (3-nitrophenyl). In this experiment, the concentrated sulfuric acid and glacial acetic acid is uesed as the reaction solvent, wherein the N-bromosuccinimide (NBS) in a slight excess, Under optimumconditions Double (3-nitro-phenyl)-4-bromo phenyl phosphine oxide in 65% yield. We use the Cross-coupling reaction way we have the 3-amino-phenyl and 4-phenyl phosphine oxide phenylacetylene. In this experiment, through the use of N-dimethylacetamide (DMAc) as a solvent, phenylacetylene (PAC), distilled under reduced pressure prior to use), bis (triphenylphosphine) palladium as a catalyst, riphenyl phosphine (PPh3) as a ligand, so iodide co-catalyst, Under optimum conditions, Double (3-nitro-phenyl)-4-phenyl acetylene phenyl phosphine oxide in 56% yield. By the reduction method using in hydrazine hydrate we creats monomer bis (3-amino-phenyl)-4-phenylacetylene phosphine oxide, Under optimum conditions, Double (3-amino-phenyl)-4-phenyl acetylene phenyl phosphine oxide in 59% yield. By infrared the spectroscopy, nuclear magnetic resonance and their structures characterized. In this thesis we carried out a detailed study on the route of their synthesis and purification process, the effects of reaction temperature, molar ratio, reaction time and other factors on the yield. By the use of Synthesis of Yamazaki, Bis (3-amino-phenyl)-4-phenylethynyl phenyl and phosphine oxide and terephthalic acid (TPA), and For stupid diamine (PPDA), The effect of the reaction solvent, reaction temperature, reaction time, several factors intrinsic viscosity aramide. The results showed that the monomer concentration is 0.35mol/L, NMP 4 times the amount of Py, the polymerization temperature is 120℃, the reaction time was 4h to obtain a polymer under the conditions of the max imumintrinsic viscosity of 0.270 (dL/ g). The intrinsic viscosity of the polymer was measured by using FT-IR,1H-NMR, 31P-NMR conducted a structural analysis of the polymers, The thermal properties of the polymer were studied by DSC. The measured tensile strength of the polymer 23.34 Mpa, elongation rate reached 1.33%, the elastic modulus of 1.9GPa. Due to show more difficult to controlthe reaction conditions, the polymerization of the polyamide film brittle. The contact anglemeasurement results show that the introduction of phenylacetylene structure such that the stiffness of the molecular chain, an amorphous layer of the diffusion pathincreases, the performance of the contact angle becomes smaller, increasing the water absorption. Ethynyl benzene structure may be introduced intothe polymer to obtain a higher flame retardance, Stability studies show that the introduction of benzene acetylene monomer structure affect stability of the polymer in concentrated sulfuric acid. |
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