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Received August 19, 2013
Accepted September 17, 2013
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N-사이크로헥실말레이미드의 합성 및 정제 입자 제조
Synthesis of N-cyclohexylmaleimide and Preparation of It’s Purified Particles
부경대학교 화학공학과, 608-739 부산시 남구 용당동 산 100
Department of Chemical Engineering, Pukyoung National University, San 100 Yongdang-dong, Nam-gu, Busan 608-739, Korea
csju@pknu.ac.kr
Korean Chemical Engineering Research, February 2014, 52(1), 40-44(5), 10.9713/kcer.2014.52.1.40 Epub 3 February 2014
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Abstract
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.
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