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2,4,6-三硝基氯苯是一种重要的医药和化工中间体,也是合成新型耐热炸药的重要原料。本文以2,4-二硝基氯苯为原料,浓硫酸与发烟硝酸体系为硝化试制备得到2,4,6-三硝基氯苯,并利用红外(IR)、核磁共振(NMR)、质谱(MS)等对产物进行了表征。研究了物料配比、反应温度、时间对硝化反应收率的影响,确定了优化的工艺条件:n(发烟硝酸)∶n(2,4-二硝基氯苯)=4.76∶1,n(浓硫酸)∶n(发烟硝酸)=4.0∶1,反应温度为130℃,反应时间为7h时,2,4,6-三硝基氯苯收率可达到84.4%,熔点为82.8℃,液相色谱分析纯度为93.4%。
2,4,6 - trinitrochlorobenzene is an important pharmaceutical and chemical intermediates, but also the synthesis of new heat-resistant explosives important raw materials. In this paper, 2,4-dinitrochlorobenzene as raw material, concentrated sulfuric acid and fuming nitric acid system for the preparation of nitrification 2,4,6-trinitrochlorobenzene, and the use of infrared (IR), nuclear magnetic resonance (NMR) , Mass spectrometry (MS), etc. The product was characterized. The effects of material ratio, reaction temperature and time on the yield of nitration reaction were studied. The optimized process conditions were as follows: n (fuming nitric acid): n (2,4-dinitrochlorobenzene) = 4.76:1, n (Concentrated sulfuric acid): n (fuming nitric acid) = 4.0:1, the reaction temperature is 130 ℃, the reaction time is 7h, the yield of 2,4,6-trinitrochlorobenzene can reach 84.4% and the melting point is 82.8 ℃ , HPLC purity was 93.4%.