アルミナ充填層反応装置によるエチレンジアミンとプロピレングリコールの反応 : 実験計画法によるメチルピペラジン収率, 最適条件の探索

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The reaction of ethylenediamine (ED) and propylene glycol was examined in the alumina-packed bed reactor. Methylpiperazine (MP) was obtained with other products (methylpyrazine, methylethylpyrazine, methylpropylpyrazine). Since this reaction mechanism is unknown, statistical method was used to find optimum conditions for the yield of methylpiperazine. The first part of the investigation consisted of central composite design. Five variables were chosen ; reaction temperature (a), catalyst weight (b), molar ratio of reactants (c), amount of water added (d), and percentage of added promotor (e). The second-order response functions were given for (1) yield of MP, (2) total yield, and (3) MP selectivity. In analysis of variance for (1) and (2), the fits of functions were reasonable. Experiments in the direction of the steepest ascent based on the second-order response function showed that the yield of MP dropped beyond 313°. It was concluded from the experimental results that the optimum conditions are as follows : (a) 312.9°, (b) 24.71 g, (c) 0.4/1.0 (ED ml/PG ml), (d) 0.853/1.0 (H_2O ml/PGI ml), and (e) 7.073%, by which the maximum yield was 45.27%.
公益社団法人日本薬学会の論文
1976-06-25