1,3-Bis(p-carboxyphenyl)-1,1,3,3,-tetramethyldisiloxane을 함유하는 새로운 폴리아미드의 합성과 성질

이수민; 김기수; 박경택

Polymer(Korea), Vol.20, No.1, 25-32, January, 1996

Export Citation

1,3-Bis(p-carboxyphenyl)-1,1,3,3,-tetramethyldisiloxane을 함유하는 새로운 폴리아미드의 합성과 성질

Synthesis and Characterization of New Polyamides Containing 1,3-Bis(p-carboxyphenyl)-1,1,3,3-tetramethyldisiloxane

이수민, 김기수, 박경택

초록

주사슬에 실리콘을 함유하는 새로운 방향족 폴리아미드를 실페닐렌/실록산기 함유 단량체와 스피로아세탈을 비롯한 다양한 방향족 단량체와의 축합중합으로 합성하였다. 이때 사용된 실페닐렌/실록산 함유 단량체 는 1,3-bis(p-chlorocarbonylphenyl)-1,1,3,3-tetramethyldisiloxane (DMCI)였다. 합성된 이들 중합체의 구조는 FT-IR, ¹H-NMR 그리고 원소분석으로 하였으며 열적 성질은 DSC와 TG.A로 측정하였다. 합성된 중합체들의 용액점성도는 0.21∼0.69 dL/g였으며 DMF, DMAc, DMSO 그리고 NMP와 같은 극성 용매에 용해되는 성질을 가졌다. 중합체의 녹음 전이온:.(T_m), 초기분해온도(IDT) 그리고 10% 질량손실온도(T₁₀)는 각각 196∼282℃, 352∼415℃ 그리고 394∼464℃였다. 고광각 X-ray 회절(WAXD) 실험 결과 PAS 시리즈 중합체는 반결정형의 구조를 소유하는 것으로 판명되었다.

New aromatic polyamides having silicon moieties in the main chain were prepared by polycondensation reaction of silphenylene/siloxane-containing monomer with spiroacetal and other aromatic monomers. The silphenylene/siloxane-containing monomer type employed was 1,3-bis(p-chlorocarbonylphenyl)-1,1,3,3-tetramethyldisiloxane (DMCL). The structures of these polymers were determined by FT-IR, ¹H-NMR and elemental analyses. Their thermal properties were characterized by DSC and TGA. The polymers had inherent viscosities in the range of 0.21∼0.69dL/g. These polymers were readily soluble in various polar solvents such as DMF, DMAc, DMSO and NMP. The melting transition (T_m), initial decomposition (IDT) and 10% weight loss temperatures (T₁₀) of these polymers were detected over the temperature range of 196∼282℃, 352∼415℃ and 394∼464℃, respectively. The structures of PAS series as determined by WAXD indicated that they were found to be semicrystalline.

Keywords:polyamide;silphenylene-siloxane polymer;silicon polymer

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[1] Cassidy PE, J. Macromol. Sci.-Chem., A15(7), 1435 (1981)

[2] Seymour RB, Kirshenbaum GS, "High Performance Polymers: Their Origin and Development," Elsevier, New York (1986)

[3] Critchley JP, Knight GJ, Wright WW, "Heat-Resistant Polymers: Technologically Useful Materials," Plenum, New York (1984)

[4] Kaito A, Kyptani M, Nakayama K, Macromolecules, 24, 3244 (1991)

[5] Frosini A, Levita G, J. Polym. Sci. B: Polym. Phys., 15, 239 (1977)

[6] Bowen HJM, "Tables of Interatomic Distances and Configurations in Molecules and Ions," Spec. Publ. 11, Chem. Soc., London (1958)

[7] Cottrell TL, "The Strength of Chemical Bonds," 2nd Ed., Butterworths, London (1958)

[8] Pauling L, "The Nature of Chemical Bond," 3rd Ed., p. 85, 189, Cornell Univ., Press, Ithaca, New York (1960)

[9] Collings WR, Chem. Eng. News, 23, 1616 (1945)

[10] Zeigler JM, Fearon FWG, "Silicon-Based Polymer Science: A Comprehensive Resource," P. 741-752, ACS, Washington D.C. (1990)

[11] Pearce E, Trans. Am. Soc. Art. Int. Org., 14, 220 (1968)

[12] Perrin DD, Armarego WLF, "Purification of Laboratory Chemicals," 3rd Ed., Pergamon Press, New York (1988)

[13] Ghatge ND, Mohite SS, Polyhedron., 6(3), 435 (1987)

[14] Kim KS, Lee SM, Ryu KC, Lee KS, Polym. Bull., 35(1-2), 57 (1995)

[15] Lee SM, Kim KS, Lee KS, Lee SK, Polym.(Korea), 13(10), 888 (1989)