Abstract:
Anthraquinone dyes are the second most important type of dyes after azo dyes. In particular, 1-aminoanthraquinone has been extensively utilized in the preparation of diverse anthraquinone dyes. This study employed a continuous-flow method to synthesize 1-aminoanthraquinone safely and efficiently through the ammonolysis of 1-nitroanthraquinone at high temperatures. Various conditions (reaction temperature, residence time, molar ratio of ammonia to 1-nitroanthraquinone (M-ratio), and water content) were investigated to explore the details of the ammonolysis reaction behavior. Operation conditions for the continuous-flow ammonolysis were optimized using Box-Behnken design in the response surface methodology, and ~88% yield of 1-aminoanthraquinone could be achieved with an M-ratio of 4.5 at 213 °C and 4.3 min. The developed process\'s reliability was evaluated by performing a 4 h process stability test. The kinetic behavior for the preparation of 1-aminoanthraquinone was investigated under continuous-flow mode to guide the reactor design and to gain a deeper understanding of the ammonolysis process.
摘要:
蒽醌染料是仅次于偶氮染料的第二重要类型的染料。特别是,1-氨基蒽醌已广泛用于制备多种蒽醌染料。本研究采用连续流方法通过高温氨解1-硝基蒽醌,安全有效地合成1-氨基蒽醌。各种条件(反应温度,停留时间,氨与1-硝基蒽醌的摩尔比(M比),和水含量)进行了研究,以探索氨解反应行为的细节。在响应面法中使用Box-Behnken设计优化了连续流氨解的操作条件,在213°C和4.3min时,M比为4.5,可获得约88%的1-氨基蒽醌产率。通过进行4小时的过程稳定性测试来评估开发过程的可靠性。在连续流模式下研究了制备1-氨基蒽醌的动力学行为,以指导反应器设计并对氨解过程有更深入的了解。