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카바모일기를 측좨로 갖는 방향족 폴리아미드의 합성 및 물성(I) -열적 및 화학적 처리에 의한 화학구조 변화-
오태진 한국섬유공학회 1995 한국섬유공학회지 Vol.32 No.4
We have successfully synthesized new aromatic polyamide having pendant amide group, i.e., aromatic poly(2,5-diaminobenzamide-terephthalamide) (PDB TA) and poly(diamino-carbamoylbenzanilide-terephthalamide) (poly(DACB-TPC)) by the low temperature solution polymerization of terephthaloyl chloride with aromatic amide diamines of 2,5-diamino-benzamide, 4,4'-diamino-6-carbamoylbenzanilide and 3,4'-diamino-6-carbamoylbenzan ilide . The changes of chemical structure along a polymer chain during thermal and chemical treatment were examined by FT-FR spectroscopy. The thermal cyclization of poly(2,5-dimino be n am ids-terephthalamide) (PDB TA) and poly(4,4'-diamino-6-carbamoylbenz anilide- terephthalamide) (poly(p-DAC B-TPC ) in the absence and in the presence of catalyst such as LiCl produces both quinazolone and benzoxazinone rings by dehydration and deamination respectively through condensation reaction of pendant carbamoyl group and amide. bond along a polymer chain. The chemical cyclization of PDBTA and polyp-DACB-TPC) in fuming H2SO4, on the contrary, produces nitril groups exclusively along a polymer chain via strong dehydration reaction of pendant carbamoyl group itself in fuming H2SO4.
카바모일기를 측쇄로 갖는 방향족 폴리아미드의 합성 및 물성(III) -열적 및 기계적 성질-
오태진,김진사,이승조,O, Tae-Jin,Kim, Jin-Sa,Lee, Seung-Jo The Korean Fiber Society 1995 한국섬유공학회지 Vol.32 No.5
The thermal stability of poly(2,5-diaminobenzamide-terephthalamideXPDB TA) and poly(4,4'-diaminocarbamoylbe- nzanilide-te.ephthalamide) poly(PDACB -TPC ) was comparable with that of poly(p-phenyleneterephthalamideXPPTA) ; The PDBTA was decomposed with slower rate and Save higher residue than PPTA. The onset temperature of decomposition of heat-treated PDBTA and poly(PDACB-TPC) as well as chemically treated(with fuming sulfuric acid) polyp-DACB-TPC) shows 520℃, 517℃ and 514℃ measured by TGA under nitrogen atmosphere with rate of 10℃/min respectively. Tensile measurement of undrawn PDBTA films heat-treated at 200℃ and 300℃, respectively, for 1 hour gives around 25kg/mm2 (250MPa) of tensile strength and 900kg/mm2(gGPa) of tensile modulus, and that of wet-drawn PDBTA films(0.7 times in machine direction) shows around 52kg/mm2(510MPa) of tensile strength and around 2500kg1mm2(250pa) of tensile modulus. Tensile properties of poly(PDACB-TPC) film prepared by using hanger type coater are superior to that obtained by casting on the 섭ass plate. The tensile properties increase with increasing draw ratio. Tensile measurement of wet-drawn poly(p DACB-TPC) fims(0.5 times in machine direction) prepared by using hanger type coater Bives around 56∼62kg/mm2(550∼608MPa) of tensile strength and around 2565kg/mm2(220pa) of tensile modulus. Dynamic mechanical measurements carried out by Rheovibron at 110Hz of both undrawn and wet-drawn PDBTA as well as poly(p-DACB-TPC) films treated at 300℃ for 1 hour represent that the aromatic polyamide film retains outstanding mechanical properties even at 400℃. The crystallinity of polyamide films was investigated by X-ray difaactovam obtained by reflection method using nickel filtered CuKa radiation, indicating that the polymer has low degree of crystallinity.
카바모일기를 측쇄로 갖는 방향족 폴리아미드의 합성 및 물성(ll) -모델 반응-
오태진,곽경진,서문호,O, Tae-Jin,Gwak, Gyeong-Jin,Seo, Mun-Ho 한국섬유공학회 1995 한국섬유공학회지 Vol.32 No.4
The changes of chemical structure along a polymer chain during thermal and chemical treatment were examined by FT-lR spenxoscopy. The thermal cyclization of poly(2,5-diaminobenzamide-terephthalamide) (PDBTA) and poly(4,4'-dia- vino-6-carbamoylbenzanilide-terephthalamide) (polyul-DACB -TPC)) in the absence and in the presence of catalyst such as LiCl produces both a large amount of quinazolone and a small a mount of benzoxazinone along a polymer chain; the amount of quinazolone and benzoxazinone formed by dehydration and deamination reaction through condensation reaction of pendant carbamoyl fyoup and amide bond along a polymer chain during thermal treatment of the polymer was determined using calibration curve obtained with the absorbance of model compounds of 6-benzoylamino-2-pheny1-4-(3H) -quinazolone and of 6-benzoylamino-2-phenyl-4H-3,1-benzoxazin-Lone measured at wavenumber of 1358 and 1742cm -1 It turns out that thermal cyclopolycondensation of PDBTA without LiCl at 270'I produces 76% of quinazolone and 24% of benzoxazione as well as with LiCl gives 89% and 11%, respectively. The chemin cyclization of PDBTA and poly(p-DACB-TPC) in fuming H2SO4, on the contrary, produces nitril groups exclusively along a polymer chain via strong dehydration reaction of carbamoyl groups along polymer chain in fuming H2SO4 ; it is confirmed by chemical treatment in fuming H2SO4 of model compound Rr, leis(2,5-N-benzoyldiamino) benzamide, which gives around 80% of bis(2,5-N-benzoyldiamino) benzonitrile, VII.
오태진,장용석 한국섬유공학회 1998 한국섬유공학회지 Vol.35 No.3
In-situ polymerized anisotropic spinning solution of poly(DACYB/TPC) was prepared by low temperature solution polymerization of DACYB and TPC in N-methyl pyrrolidone with addition of equimolar amount of $Li_2CO_3$, which was directly dry-jet wet spun to give high strength (higher than 20 g/d) and high modulus (higher than 720 g/d) aromatic polyamide fiber. Mechanical properties of the fiber was strongly dependent on the dry-jet wet spinning conditions, i.e., spinneret diameter, spin draw ratio, air gap and heat treatment conditions (temperature and tension). Poly(DACYB/TPC) fiber spun through spinning holes with diameter 0.06 mm had higher tensile property than the fiber spun with diameter 0.15 mm at the same spin draw ratio, The latter, however, had higher tensile property than the former at the identical fiber thickness. Fibers prepared by dry-jet wet spinning through the air gap of around 40 mm gave the best properties by enhancing spin draw ratio. Heat treatment (above 25$0^{\circ}C$) under tension (higher than 2 g/d) improved the tensile property of poly(DACYB/TPC) fiber, particularly in tensile modulus.