超音速气流固相反应合成对二甲胺基苯甲醛缩对氨基苯甲酸Schiff碱

Solid-State Synthesis of Schiff Base Derived from p-Dimethylaminobenzaldehyde and p-Aminobenzoic Acid with Supersonic Speed Airflow

在自制的超音速气流固相反应装置中,以对二甲胺基苯甲醛和对氨基苯甲酸为原料合成了对二甲胺基苯甲醛缩对氨基苯甲酸 Schiff 碱。特点是采用超音速气流使对二甲胺基苯甲醛和对氨基苯甲酸在反应器中摩擦活化,再通过撞击固定靶产生快速的能量转换而发生化学反应。用傅里叶变换红外光谱、核磁共振、质谱等方法对产物进行了表征,考察了循环反应次数和反应压力对产物收率的影响。实验结果表明,对二甲胺基苯甲醛缩对氨基苯甲酸 Schiff 碱适宜的反应条件为:n(对二甲胺基苯甲醛):n(对氨基苯甲酸)=1:1,反应压力0.4 SPa,循环反应次数5次。在此条件下,原料的转化率达100%,产物收率为92.45%。

A Schiff base derived from p-dimethylaminobenzaldehyde and p-aminobenzoic acid was prepared in self-designed solid-state reaction devices with supersonic speed airflow. By aid of supersonic speed airflow the particles of feed mixture in reaction zone with friction against each other activate, impact on a certain target, initiate a rapid exchange of energy and react. The stream goes through the circulation collecting system. The procedure is repeated several times to gain the yield. Schiff base can be thus prepared by solid-state reaction in supersonic speed airflow successfully. The structure of product was characterized by means of FTIR, 1^H NMR, MS. Effects of reaction times and pressure on product yield were further studied. When pressure 0.4 MPa and through 6 times of reactive impact, conversion is 100% and yield is 92.45%. Schiff base can be prepared by solid-state reaction in supersonic speed airflow. This method is feasible and has particular advantages： simple manipulation, short operation time, high productivity.