微波辐射下SO_4^(2-)/ZrO_2-TiO_2催化合成乙酸诺卜酯

Synthesis of Nopyl Acetate Catalyzed by SO_4^(2-)/ZrO_2-TiO_2 under Microwave Irradiation

以自制诺卜醇和乙酸为原料,固体超强酸SO42-/ZrO2-TiO2为催化剂,甲苯为带水剂,在微波辐射条件下合成乙酸诺卜酯,考察了微波辐射条件和催化剂制备条件、催化剂用量等对乙酸诺卜酯得率的影响。结果表明,微波辐射温度、时间及催化剂的制备条件和用量对乙酸诺卜酯得率有较大影响。优化的工艺条件为:诺卜醇质量20g,醇酸物质的量比1∶1.15,微波辐射温度105℃,微波功率650W,辐射时间85min,催化剂SO42-/ZrO2-TiO2(Ti与Zr质量之比为6∶1,焙烧温度450℃)用量为诺卜醇质量的2.5(,该条件下乙酸诺卜酯得率81.3。(此外,催化剂可重复使用4次。与普通加热反应相比,时间缩短,产物得率提高。

Nopyl acetate was synthesized by nopol and acetic acid under microwave irradiation and catalyzed by solid superacid SO4^2-/ZrO2-TiO2. The influences of various reaction parameters, such as irradiation temperature, time, power, conditions for preparation of catalyst and catalyst dosage were investigated. Results show the proper technological conditions as follows ： irradiation temperature 105℃, irradiation time 85 min, microwave power 650 W, catalyst type Ti ： Zr 6 ： 1, calcination temperature 450℃ and solid superacid dosage 2.5 % （ based on nopol mass）. Under this condition, the yield of nopyl acetate reached 81.3%. Furthermore, the regenerated catalyst could be repeatedly used for 4 times.