N-사이크로헥실말레이미드의 합성 및 정제 입자 제조

문부현; 주창식; Bu-Hyun Moon; Chang-Sik Ju

Korean Chemical Engineering Research, Vol.52, No.1, 40-44, February, 2014

Export Citation

N-사이크로헥실말레이미드의 합성 및 정제 입자 제조

Synthesis of N-cyclohexylmaleimide and Preparation of It’s Purified Particles

문부현, 주창식 ^†

부경대학교 화학공학과, 608-739 부산시 남구 용당동 산 100

Bu-Hyun Moon, and Chang-Sik Ju^†

Department of Chemical Engineering, Pukyoung National University, San 100 Yongdang-dong, Nam-gu, Busan 608-739, Korea

E-mail:

초록

고순도의 CHMI 입자를 제조하는 공정을 개발하기 위해서, CHMAIE로부터 CHMI를 합성하고 정제한 후 형상화하는 공정 전반에 대한 실험적 연구를 수행하였다. CHMI 합성에 있어서는 n-헵탄 환류 이미드화 반응이 톨루엔 put-out 이미드화 반응보다 CHMI의 평형 전화율이 높을 뿐 아니라, CHMI의 석출공정에도 유리한 것으로 나타났다. 합성된 CHMI를 n-헵탄으로 2회 세척하면 11.7%의 무게 감소율이 발생하지만, 99.7%의 고순도 CHMI를 얻을 수 있었다. CHMI 입자의 제조에서는 3 mm 나선형 노즐을 통하여 1.5~2.0 kg/cm2의 압력으로 CHMI 용융액을 토출시키면 가장 효과적으로 CHMI 입자를 제조할 수 있었다.

For the purpose of development of an effective process for purified CHMI particles, a series of experimental researches on the synthesis of CHMI from CHMAIE, purification and precipitation of CHMI were preformed. It is turned out that n-heptane reflux imidation is more beneficial than toluene put-out imidation not only to the synthesis but to the precipitation of CHMI. By washing the synthetic CHMI with cold n-heptane twice, purified CHMI with 99.7% purity could be obtained at the cost of 11.7% weight loss. And CMHI particles were effectively prepared by spouting molten CHMI through the spiral nozzle with 3 mm diameter under the pressure of 1.5~2.0 kg/cm2.

Keywords:CHMI;CHMAIE;Synthesis;Imidation;Particle

[References]

Yuksei M, Canak TC, Serhatli IE, Polym. for Adv. Technol., 20(3), 312 (2009)
Kim NS, Nam BW, J. Ind. Eng. Chem., 13(2), 221 (2009)
Yang L, Sun D, J. Appl. Polym. Sci., 100(2), 918 (2007)
Song KD, Li HM, J. Macromoleculear Sci., 42(6), 741 (2005)
Sun DH, Wang B, He J, Zhang R, Liu ZM, Han BX, Ying HA, Polymer, 45(11), 3805 (2004)
Nakano T, Yade T, Kobunshi Ronbunshu, 61(4), 282 (2004)
Gau J, Hu X, Yang L, Polym.-Plast. Technol. Eng., 43(2), 463 (2004)
Yang LT, Sun DH, Li YF, Liu GD, Gao JG, J. Appl. Polym. Sci., 84(5), 1070 (2002)
Yoon WJ, Kim YS, Kim IS, Choi KY, Korean J. Chem. Eng., 21(1), 147 (2004)
ゴムプラスチック配合藥品, 株式會社ラバ-タイジェスト社, 425 (2003)
Jing S, Hua KG, Li G, Lin WD, Chem. Eng. of Oil and Gas., 37(4), 337 (2008)
Song KD, Li HM, Chinese J. of Synthetic Chem., 12(4), 372 (2004)
Kita Y, Kishino K, Nakagawa K, J. Appl. Polym. Sci., 63(3), 363 (1997)
Moon BH, Ju CS, “Developnent of a Synthetic Process for N-cyclohexylmaleiamic Acid Isobutyl Ester,” Korean. Chem. Eng. Res.(HWAHAK KONGHAK), in Press.

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[1] Yuksei M, Canak TC, Serhatli IE, Polym. for Adv. Technol., 20(3), 312 (2009)

[2] Kim NS, Nam BW, J. Ind. Eng. Chem., 13(2), 221 (2009)

[3] Yang L, Sun D, J. Appl. Polym. Sci., 100(2), 918 (2007)

[4] Song KD, Li HM, J. Macromoleculear Sci., 42(6), 741 (2005)

[5] Sun DH, Wang B, He J, Zhang R, Liu ZM, Han BX, Ying HA, Polymer, 45(11), 3805 (2004)

[6] Nakano T, Yade T, Kobunshi Ronbunshu, 61(4), 282 (2004)

[7] Gau J, Hu X, Yang L, Polym.-Plast. Technol. Eng., 43(2), 463 (2004)

[8] Yang LT, Sun DH, Li YF, Liu GD, Gao JG, J. Appl. Polym. Sci., 84(5), 1070 (2002)

[9] Yoon WJ, Kim YS, Kim IS, Choi KY, Korean J. Chem. Eng., 21(1), 147 (2004)

[10] ゴムプラスチック配合藥品, 株式會社ラバ-タイジェスト社, 425 (2003)

[11] Jing S, Hua KG, Li G, Lin WD, Chem. Eng. of Oil and Gas., 37(4), 337 (2008)

[12] Song KD, Li HM, Chinese J. of Synthetic Chem., 12(4), 372 (2004)

[13] Kita Y, Kishino K, Nakagawa K, J. Appl. Polym. Sci., 63(3), 363 (1997)

[14] Moon BH, Ju CS, “Developnent of a Synthetic Process for N-cyclohexylmaleiamic Acid Isobutyl Ester,” Korean. Chem. Eng. Res.(HWAHAK KONGHAK), in Press.