Search / Korean Journal of Chemical Engineering
HWAHAK KONGHAK,
Vol.29, No.2, 199-205, 1991
유동층 반응기를 이용한 Isophthalonitrile로부터 Tetrachloroisophthalonitrile의 합성에 관한 연구
A Study on the Synthesis of Tetrachloroisophthalonitrile from Isophthalonitrile in a Fluidized Bed Reactor
Isophthalonitrile(IPN)을 염소화하여 Tetrachloroisophthalonitrile(TPN)을 합성하는 반응의 거시적인 반응기구 및 반응속도를 연구하고 아울러 유동층 반응기를 이용하여 TPN을 합성하기 위한 반응기의 설계 및 조작조건들을 구하였다. 고정층 반응기를 이용하여 얻은 실험치와 이론치를 비교함으로서 TPN의 합성반응은 각단계가 의 1차반응인 연속반응임을 알았으며 반응기의 온도가 300℃ 때의 속도상수를 구하였다. 유동층 반응기의 설계 및 조업에 필요한 기본 데이터들을 얻기 위하여 입경과 조업 온도에 따른 촉매의 최소 유동화속도를 조사하였으며 이를 기본으로 하여 설계 제작한 벤치 스케일 유동층 반응기에서 -70+100mesh의 30wt% FeCl3/활성탄 촉매를 사용하여 순도 95% 이상의 TPN을 합성하기 위한 Cl2/IPN의 몰비, 반응온도, 체재시간 및 유동층의 H/D의 값 등을 결정하였다.
Macroscopic reaction kinetics of the chlorination reaction of isophthalonitrile(IPN) to produce tetrachloroisophthalonitrile(TPN) was studied and the optimal design and operating conditions of a fluidized bed reactor for the chlorination of IPN were investigated experimentally. Comparing the experimental data obtained from a fixed bed reactor with the theoretical ones, the IPN→X→TPN type consecutive reaction mechanisms and pseudo-first order reaction rate for each step were found satisfactory and the kinetic rate constants for each step at 300℃ were obtained. Experiments were conducted in a lab-scale fluidized bed column in order to obtain the information on the minimum fluidizing velocity of catalyst which in turn served as the basis for the design and operation of a bench-scale fluidized bed reactor. The chlorination reactions were undertaken in this reactor using the 30wt% FeCl3/activated carbon particles of -70+100 mesh sizes as the catalyst to determine the optimal operating conditions for the production of TPN of purity greater than 95%, which include temperature, molar ratio of Cl2/IPN in the feed and mean residence time. Optimal H/D ratio was proposed also for the design.
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