유동층반응기에서 Hexachlorocyclopentadiene의 합성

조철군; 우제완; 김종수; 신용우

Journal of the Korean Industrial and Engineering Chemistry, Vol.6, No.4, 664-672, August, 1995

Export Citation

유동층반응기에서 Hexachlorocyclopentadiene의 합성

Synthesis of Hexachlorocyclopentadiene in a Fluidized Bed Reactor

조철군, 우제완, 김종수, 신용우

초록

유동층반응기를 사용하여 유기염소계 농약의 원료인 Hexachlorocyclopentadiene(HCCP)을 합성하였다. 활성탄 촉매가 유동화되고 있는 벤치규모의 반응기에서 Dicyclopentadiene(DCP)을 염소화시켜 HCCP를 합성하였으며, 반응온도, 염소/DCP 몰비 및 공간시간을 실험인자로 선정하여 공업용 유동층반응기에 기준한 합성조건과 유동특성을 실험으로 결정하였다. 최적 합성조건은 반응온도 380℃, 염소DCP 몰비 13.5, 공간시간 7초이었고, 이때 유동층의 길이는 50∼55cm, 유동화유속/최소유동화 유속의 비는 2, 유동층길이/직경비가 6∼7인 유동특성을 보여 주었으며, HCCP의 선택도는 87%이었고 합성수율은 85%이었다.

Hexachlorocyclopentadiene(HCCP), which is a raw material of organochloro agrochemicals, was synthesized by the chlorination of dicyclopentadiene(DCP) in a bench-scale fluidized bed reactor packed with active charcoals as catalyst. With the requirements for the industrial scale reactor taken into consideration, optimum synthetic conditions and fluidization characteristics were experimentally determined. It was shown that the selectivity to and yield of HCCP were 87% and 85%, respectively, when reaction temperature is 380℃, a mole ratio of chlorine to DCP 13.5, space time 7sec, bed length 50∼55cm, a ratio of fluidization velocity to minimum fluidization velocity 2, and a ratio of bed length to bed diameter 6∼7.

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[1] Scheelline HW, "Flame Retardant Additives," Stanford Research Institute Report No. 92, Process Economics Program, Menlo Park, California, U.S.A. (1975)

[2] Brown J, "Kirk-Othmer Encyclopedia of Chemical Technology," 3rd ed., 5, 791 (1979)

[3] Hanna DL, Rudnitzki AJ, U.S. Patent, 3,073,869 (1963)

[4] Downes HI, De Bataafsche Petroleum, Brit. Patent, 771,650 (1957)

[5] Maude AH, Rosenberg DS, U.S. Patent, 2,650,942 (1953)

[6] Maude AH, Rosenberg DS, U.S. Patent, 2,714,124 (1955)

[7] Minsinger M, U.S. Patent, 3,364,269 (1968)

[8] Kenneth K, Trenton A, McMaster AL, U.S. Patent, 3,649,699 (1972)

[9] Steinhofer A, Minsinger M, U.S. Patent, 2,945,893 (1960)

[10] Lim BK, Ju DP, Kim C, HWAHAK KONGHAK, 29(2), 199 (1991)

[11] Lidov RE, U.S. Patent, 2,900,402 (1959)

[12] Breitmaier E, Voelter W, "Carbon-13 NMR Spectroscopy," 3rd ed., VCH, Weinheim, Germany (1989)

[13] Kunii D, Levenspiel O, "Fluidization Engineering," 2nd ed., Butterworth-Heinemann, MA, U.S.A. (1991)