초록
본 논문은 DNAM(Dinitroammeline)합성공정 개발을 위한 Lab scale 합성 과정을 소개하고 분석결과를 기록한 것으로 주요 내용은 다음과 같다 Melamine을 출발물질로 하여 니트로화와 산화 반응을 통해 DNAM을 합성하였다. 수율과 순도의 최적 조건을 찾기 위해 투입순서, 반응시간, 반응물 당량 등을 변경하여 실험을 수행하였다. DNAM 합성의 최적화된 조건은 3시간에서 3시간 30분 정도 반응시간이고, 니트로화 혼합물의 무게비는 1:1.4(아세트산 무수물:농질산)이며, 최종 수율은 60% 이상이다.
We studied the Lab-scale process for the development of DNAM in aspect of safety and overall efficiency. Melamine is used for starting material of process, DNAM was synthesized by oxidation and nitration reaction. In order to optimize the process parameters with the product in higher yield and purity, a systematic study with variation of different parameters like molar ratio of nitrating mixture, conditioning time and order of reactant was carried out. The optimized reaction conditions for the synthesis of DNAM were : conditioning time of $3{\pm}3.5$ hour and nitrating mixture in 1:1.4 molar ratio. In order to proceed a stable reaction, melamine was added with enough time to relieve reaction heat. From these reaction condition, DNAM could be obtained in a yield of more than 60%.
