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Research on the Prepration of 2, 4 (2,6)-Dimethyl Nitrobenzene by m-Xylene Nitrating

Author: LiYongChang
Tutor: YangASan；YuJianWei
School: Zhejiang University of Technology
Course: Chemical Engineering
Keywords: 2,4 ( 2,6) - dimethyl- nitrobenzene M-xylene Nitrification Distillation Second nitro compounds
CLC: TQ246.1
Type: Master's thesis
Year: 2009
Downloads: 22
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Abstract


Verified a small test the reliability of the technology in a Research Institute of Chemical Industry, based on small test technology for the design of the pilot plant, to carry out pilot studies, and for the nitration of m-xylene the dinitro content test results high situation, further development of the m-xylene nitration conditions to optimize the work of a small pilot study, and achieved significant results in the reduction of the proportion of the two nitro compounds generated. Nitration of m-xylene, distillation pilot study shows that, compared to 2.68, mixed acid FNA71%, nitric acid ratio of 1.0, the the nitration temperature of 12 to 15 ° C, under the conditions of the reaction time of 3 to 4 hours, m-xylene average conversion rate of 96.75%; nitration product of 2,4 - dimethyl-nitrobenzene and 2,6 - dimethylnitrobenzene generation ratio of 82:18; nitrification process, 2,4 (2,6) - dimethylnitrobenzene average closing 95.61% the the dinitro content up to 1.5 to 4.0%; compared and FNA of the formation of the dinitro was to play a leading role; increase compared to reduce FNA help to reduce the nitro compounds nitrites content. Batch distillation separation of 6.4 meters high CY-700 filler xylene nitro compounds, a reflux ratio of about 12, the 2,4 - and 2,6 - dimethylnitrobenzene content can reach more than 99%; Distillation process, resulting in the loss of 2,4 - dimethyl-nitrobenzene mainly due to the losses caused by the retirement of the the distillation kettle residual tar distillation process 2,4 (2,6) - dimethylnitrobenzene closing rate of 89.65%. M-xylene nitration conditions to optimize small pilot study showed that the most significant factor affecting the production amount of dinitro acid mixture by FNA. FNA lower, the generation amount of the two nitro less; followed compared compared to larger, the two nitro generating less amount; meta-xylene conversion rate increased with the nitration temperature increases, 2, 4 (2,6) - dimethylnitrobenzene yield increases with the nitration temperature is decreased Jiaoyou Sheng as the amount increases with the nitration temperature increases. Given prone, m-xylene, nitration, also prone series nitrification proposed in this paper does not seek high-way conversion rate for the sake of the high selectivity of the idea, it is recommended that suitable nitration conditions: the the nitrification activity factors (FNA) 68%, compared to of 4.5, the nitration temperature 10 to 15 ° C, the the nitration reaction time for 3h. Under this condition, the meta-xylene conversion rates above 75%, 2,4 (2,6) - dimethylnitrobenzene overall yield of up to more than 97% 2,4 - dimethylnitrobenzene the proportion of 2,6 - dimethyl-nitrobenzene generating approximately i.e. 81.8:18.2, the total content of the two nitro may be controlled at 0.6% or less, the integrated factor ψ is up to more than 30; pilot conditions, di-nitro compounds the total content of up to a range of 1.5 to 4.0%, the integrated factor ψ is only 4 to 15, the formation ratio of the two nitro significantly reduced compared with the conditions in a pilot.

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