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납사분해공정 잔사유로부터 등방성/이방성 핏치의 제조
Preparation of Anisotropic/Isotropic Pitches from NCC-PFO
HWAHAK KONGHAK, October 1995, 33(5), 551-558(8), NONE
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Abstract
납사분해공정(NCC) 잔사유인 PFO 내에 잔존하는 경질의 휘발성유분을 제거하기 위하여 일차로 질소 분위기, 300℃에서 2시간 동안 열처리 과정을 수행하였다. 원료 PFO로부터 경질유분이 제거된 비휘발성의 전구체 핏치를 350℃에서 450℃의 온도 범위에서 3시간 동안 500 cc/min의 질소 분위기로 2차 열처리 과정을 거쳐 건류하였다. 370℃의 건류 온도에서 연화점 255℃, 톨루엔 불용분 28wt%의 방사 가능한 등방성 핏치를 얻었으며 이를 모세관 형태의 0.5mm 방사 구멍을 통해 방사한후 산화 밑 탄화과정을 거쳐 25㎛ 굵기의 등방성 탄소 섬유를 얻을 수 있었다. 390℃에서 건류된 핏치로부터 메조페이스 형태의 소구체가 관찰되기 시작하였으며 430℃와 450℃에서 건류된 이방성 핏치로부터는 비교적 잘 발달된 흐름 섬유상 구조의 메조페이스가 전체적으로 관찰되었다.
PFO(pyrolized fuel oil), which is the bottom oil from a NCC(naphtha cracking center), was initially heat-treated at 300℃ for 2hr under N2 blowing to remove the volatile matters from the original constituents of the feedstock. The nonvolatile precursor-pitch derived from the PFO raw material was thermally pyrolized in the temperature ranges from 350℃ to 450℃ for 3 hr during the second thermal stage under 500cc/min N2 blowing. Spinnable isotropic pitch with the softening point of 255℃ and the toluene insolubles of 28wt% was obtained at 370℃, and then was successfully spun through a 0.5mm capillary sized-spinneret. After spinning, an isotropic carbon fiber of 25㎛ diameter was obtained via oxidation and carbonization procedures. Mesophase spherules began to be observed from the second-stage product pitch pyrolized at 410℃, and bulk mesophase with a flow texture was observed at 430℃ and 450℃.
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