폴리아미드 섬유의 합성과 그 특성

이상국

Polymer(Korea), Vol.19, No.6, 779-788, November, 1995

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폴리아미드 섬유의 합성과 그 특성

Synthesis and Characterization of Polyimide Fibers

이상국

초록

p-Chlorophenol 용제를 사용하여 1단계 방법으로 3,3'-dimethy1-4,4'-diaminobiphenyl(OTOL)와 3,3',4,4'-biphenyltetra-carboxylic dianhydride(BPDA), 그리고 두 단량체, 4,4'-diaminodiphenyl ether(ODA)와 2,2'-bis(trifluoromethyl)-4,4'-diaminobipheny1(PFMB)를 사용하여, p-chlorophenol에 녹는 여러가지 공중합체를 만들었다. 첫번째 단량체로 만든 공중합체의 점도는 4.35∼5.43 dL/g였다. 이 공중합체 용액을 방사하여 섬유를 만들었으며 이들의 인장강도는 7.67∼16.28 g/d였다. 두번째 단량체를 만든 공중합체의 점도는 3.48∼6.98 dL/g 였고, 이공중합체 용액을 방사하여 만든 섬유의 최고 인장강도는 15.10 g/d, 최대 탄성율의 값은 810g/d 였다.

The random copolymerization of 3,3'-dimethy1-4,4'-diaminobiphenyl (OTOL) and 3,3', 4,4'-biphenyltetra-carboxylic dianhydride (BPDA) with two comonomers, j.e., 4,4'-diaminodiphenyl ether (ODA) and 2,2'-bis(trifluoromethy1)-4,4'-diaminobipheny1 (PFMB), was carried out using the one-step method in p-chlorophenol. Several copolymers were obtained that were soluble in p-chlorophenol. In the first series the copolymers' intrinsic viscosities ranged from 4.35 to 5.43 dL/g. The copolymers were dry-jet wet spun into fibers directly from their polymerization mixtures. The fibers were drawn to higher draw ratios of 4.5 to 6.0. The tensile strengths of the fibers were between 7.67 and 16.28 g/d. The second polymers had intrinsic viscosities of 3.48 to 6.98 dL/g. The draw ratios of fibers were much increased. Fibers of the copolymers displayed tensile strengths as high as 15.10 g/d and moduli as high as 810 g/d.

Keywords:polyimide fibers;dry-jet wet;tensile strength;nodulus;copolymerization

[References]

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Bessonov MI, Koton MM, Kudryavtsev VV, Laius LA, "Polyimides: Thermally Stable Polymers," 2nd ed., Plenum, New York (1987)
Grubb DT, Mita I, Yoon DY, "Materials Science of High Temperature Polymers for Microelectronics," vol. 227, Pittsburgh, Material Research Society (1991)
Wilson D, Stenzenberger HD, Hergenrother PM, "Polyimides," Blackie & Son Ltd., New York (1990)
Feger CJ, Khojasteh MM, McGrath JE, "Polyimides: Materials, Chemistry, and Characterization," Elsevier Science Publishers B.V., Amsterdam, N.Y. (1989)
Lupinski JH, Moore RS, "Polymeric Materials for Electrics Packaging and Interconnection," ACS Symposium Series 407, American Chemical Society, Washington, D.C. (1989)
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E.I. Du Pont de Nemours and Co.
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Koton MM, Br. Patent, 1,183,306 (1970)
Koton MM, Br. Patent, 2,025,311 (1980)
JindaD, Matsuda T, Sakamoto K, Sen-I Gakkaishi, 40(12), 42 (1984)
Alberino LM, Farrissey WJ, Rose JS, U.S. Patent, 3,708,458 (1973)
Farrissey WJ, Onder BK, U.S. Patent, 3,985,934 (1976)
Makino H, Kusuki Y, Harada T, Shimazaki H, U.S. Patent, 4,370,290 (1983)
Sasaki T, Hatani H, Kashima M, Yoshimoto H, Sasaki Y, U.S. Patent, 4,247,443 (1981)
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Rogers HG, Gaudiana RA, Hoolinsed WC, Kalyanarman PS, Manello JS, McGowan C, Sahatjian R, Macromolecules, 18, 1058 (1985)
DeTar DF, J. Org. Chem., 45, 5166 (1980)
DeTar DF, J. Am. Chem. Soc., 102, 7988 (1980)

[1] Mittal KL, "Polyimides: Synthesis, Characterization, and Applications," vol. 1 & 2, Plenum, New York (1984)

[2] Bessonov MI, Koton MM, Kudryavtsev VV, Laius LA, "Polyimides: Thermally Stable Polymers," 2nd ed., Plenum, New York (1987)

[3] Grubb DT, Mita I, Yoon DY, "Materials Science of High Temperature Polymers for Microelectronics," vol. 227, Pittsburgh, Material Research Society (1991)

[4] Wilson D, Stenzenberger HD, Hergenrother PM, "Polyimides," Blackie & Son Ltd., New York (1990)

[5] Feger CJ, Khojasteh MM, McGrath JE, "Polyimides: Materials, Chemistry, and Characterization," Elsevier Science Publishers B.V., Amsterdam, N.Y. (1989)

[6] Lupinski JH, Moore RS, "Polymeric Materials for Electrics Packaging and Interconnection," ACS Symposium Series 407, American Chemical Society, Washington, D.C. (1989)

[7] Sroog CE, Prog. Polym. Sci., 16(4), 561 (1991)

[8] E.I. Du Pont de Nemours and Co.

[9] Irwin RS, Smullen CE, U.S. Patent, 4,640,972 (1987)

[10] Koton MM, Br. Patent, 1,183,306 (1970)

[11] Koton MM, Br. Patent, 2,025,311 (1980)

[12] JindaD, Matsuda T, Sakamoto K, Sen-I Gakkaishi, 40(12), 42 (1984)

[13] Alberino LM, Farrissey WJ, Rose JS, U.S. Patent, 3,708,458 (1973)

[14] Farrissey WJ, Onder BK, U.S. Patent, 3,985,934 (1976)

[15] Makino H, Kusuki Y, Harada T, Shimazaki H, U.S. Patent, 4,370,290 (1983)

[16] Sasaki T, Hatani H, Kashima M, Yoshimoto H, Sasaki Y, U.S. Patent, 4,247,443 (1981)

[17] Kaneda T, Katsura T, Nakagawa K, Makino H, Horio M, J. Appl. Polym. Sci., 32, 3138 (1986)

[18] Lee S, Haris FW, Polymer, to submitted (1995)

[19] Rogers HG, Gaudiana RA, Hoolinsed WC, Kalyanarman PS, Manello JS, McGowan C, Sahatjian R, Macromolecules, 18, 1058 (1985)

[20] DeTar DF, J. Org. Chem., 45, 5166 (1980)

[21] DeTar DF, J. Am. Chem. Soc., 102, 7988 (1980)