MCTC(Maleic Methyl Cyclohexen Tetracarboxylic Anhydride)를 함유하는 폴리이미드의 합성과 물성

이영철; 박민규; 한상규; 정화진

Polymer(Korea), Vol.18, No.6, 899-905, November, 1994

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MCTC(Maleic Methyl Cyclohexen Tetracarboxylic Anhydride)를 함유하는 폴리이미드의 합성과 물성

Synthesis and Characterization of Polyimides Containing MCTC (Maleic Methyl Cyclohexen Tetracarboxylic Anhydride) Unit

이영철, 박민규, 한상규, 정화진

초록

MCTC(Maleic Methyl Cyclohexen Tetracarboxylic Anhydride)가 Dianhydride 성분으로 함유된 6가지의 폴리이미드 삼원공중합체를 직접중합 이미드화법으로 합성하였다. 합성된 폴리이미드의 이미드화는 FT-IR로 확인하였고 본성점도(η_inh)는 0.54-0.70dl/g이었다. 단일결합으로 연결되어 있는 MCTC 구조로 인하여 합성된 주쇄에 불규칙성을 증가시킴과 동시에 분자간 충진성을 감소시켜 무정형의 폴리이미드가 얻어졌으며 유기용매에 대한 용해성이 높았다. Poly(PMDA/MCTC-ODA)와 poly(BTDA/MCTC-ODA)의 경우 Dianhydride 성분에 대한 MCTC의 mole분율이 각각 0.9, 0.8이상에서 NMP, m-cresol, DMSO등 일반유기용매에 용해되었다. 또한 poly(MCTC/DSDA-ODA), poly(MCTC/DSDA-OTB), poly(MCTC-ODA/TPE-R), poly(MCTC-OTB/TPE-R)도 상기 유기용매에 용해되었고 N₂분위기에서의 10% 중량 감소 온도가 407℃이상으로 내열성이 높았다. 이들 폴리이미드의 인장강도 및 탄성율은 각각 58∼85MPa, 1.9∼2.6GPa로 엔지니어링 플라스틱 수준으로 높았다.

Six 3-component polyimides containing MCTC(Maleic methyl cyclohexen tetracarboxylic anhydride) unit have been synthesized using the one-step method and characterized. Imidization of the polyimides has been confirmed by FT-IR and the inherent viscosities of the polyimides were 0.54∼0.70dl/g. Due to the MCTC chemical structure which has a sing1e bond between two bulky cyclic groups, the main chain of the polyimides seems to be flexible and assymetric. Therefore, the polyimides were found to be amorphous as evidenced by the X-ray diffraction studies. When the mole fraction of MCTC in poly(PMDA/MCTC-ODA) and poly(BTDA/MCTC-ODA) are more than 0.9 and 0.8 respectively, the polylmides were soluble in various common organic solvents including NMP, m-cresol, DMAc and DMF. Poly(MCTC/DSDA-ODA), poly(MCTC/DSDA-OTB), poly(MCTC-ODA/TPE-R) and poly(MCTC-OTB/TPE-R) are also soluble in the above-mentioned organic solvents, and their 10% wt-loss temperatures in nitrogen were higher than 407℃. The tensile modulus and strength of the polyimides containing MCTC were found to be as high as those of a typical engineering plastic.

Keywords:polyimide;MCTC(Maleic Methyl Cyclohexen Tetracarboxylic Anhydride);synthesis;thermal property;mechanical property

[References]

Harris FW, Feld WA, Lanier LH, J. Appl. Polym. Sci. Appl. Polym. Symp., 26, 421 (1975)
Sroog CE, J. Polym. Sci. A: Polym. Chem., 3, 1373 (1965)
Sroog CE, J. Polym. Sci. Macromol. Rev., 11, 161 (1976)
Imai Y, Sen-I Gakkaishi, 35, 370 (1979)
Lee Y, unpublished results
Hedrick JL, Labadie JW, Palmer TD, Russell TP, "Polyimides: Materials, Chemistry and Characterization," Eds. by C. Feger, N.M. Khojasteh,and J.E. McGrath, p. 61, Elsevier, Amsterdam (1989)
Kawashima Y, Iketa T, Kitagawa H, "Polyimides: Materials, Chemistry and Characterization," Eds. by C.Feger, M.M. Khojasteh, and J.E. McGrath, p. 123, Elsevier, Amsterdam (1989)
Mita I, Kochi M, Hasegawa M, Iikuka T, Soma H, Yokota R, Horiuchi R, "Polyimides: Materials, Chemistry and Characterization," Eds. by C.Feger, M.M. Khojasteh, and J.E. McGrath, p. 123, Elsevier, Amsterdam (1989)

[1] Harris FW, Feld WA, Lanier LH, J. Appl. Polym. Sci. Appl. Polym. Symp., 26, 421 (1975)

[2] Sroog CE, J. Polym. Sci. A: Polym. Chem., 3, 1373 (1965)

[3] Sroog CE, J. Polym. Sci. Macromol. Rev., 11, 161 (1976)

[4] Imai Y, Sen-I Gakkaishi, 35, 370 (1979)

[5] Lee Y, unpublished results

[6] Hedrick JL, Labadie JW, Palmer TD, Russell TP, "Polyimides: Materials, Chemistry and Characterization," Eds. by C. Feger, N.M. Khojasteh,and J.E. McGrath, p. 61, Elsevier, Amsterdam (1989)

[7] Kawashima Y, Iketa T, Kitagawa H, "Polyimides: Materials, Chemistry and Characterization," Eds. by C.Feger, M.M. Khojasteh, and J.E. McGrath, p. 123, Elsevier, Amsterdam (1989)

[8] Mita I, Kochi M, Hasegawa M, Iikuka T, Soma H, Yokota R, Horiuchi R, "Polyimides: Materials, Chemistry and Characterization," Eds. by C.Feger, M.M. Khojasteh, and J.E. McGrath, p. 123, Elsevier, Amsterdam (1989)