超音速气流低热固相反应合成对硝基苯甲醛缩对氨基苯甲酸Schiff碱

Solid-state synthesis of Schiff base derived from p-nitrobenzaldehyde and p-aminobenzoic acid at supersonic speed airflow and low-heating temperature

为了实现无溶剂制备及缩短反应时间,研究了在超音速气流下低热固相反应制备Schiff碱。采用超音速气流使对硝基苯甲醛和对氨基苯甲酸在反应腔中摩擦活化,再通过撞击固定靶产生迅速的能量转换而发生化学反应,成功实现了超音速气流低热固相反应制备对硝基苯甲醛缩对氨基苯甲酸Schiff碱。应用FT-IR,1H NMR,MS等现代测试手段表征了产物结构。进一步讨论了循环次数以及反应压力对产物产率的影响,在反应压力0.2 MPa下,原料循环反应3次转化率即达100%。试验表明超音速气流低热固相反应能用于Schiff碱的制备,方法原理可行,并且工艺简单,反应时间短,产率高。

The solid-state synthesis of Schiff base was studied at supersonic speed airflow and low-heating temperature in order to realize solvent-free synthesis and reducing of reaction time. When the supersonic speed airflow acted on p-nitrobenzaldehyde and p-aminobenzoic acid in reaction zone, the mixture was fractioned and activated; then the mixture could react according to the exchange of rapid energy through impacting on the certain target, and Schiff base was prepared successfully by solid-state reaction at supersonic speed airflow and low-heating temperature. The structure of product was characterized by FT-IR, ^1H NMR, MS. The influence of the reaction frequency and reaction pressure on the yields of product was further studied. The yield achieved 100% after 3 times cyclic reaction under the pressure of 0.2 MPa. The results show that solid-state reaction at supersonic speed airflow and low-heating temperature can be used for the preparation of Schiff base. This method is feasible and featured by simple process, short reaction time and high productivity.