Synthesis of Nopyl Acetate Catalyzed by SO42-/ZrO2-TiO2 under Microwave Irradiation
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摘要:
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.
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关键词:
- 乙酸诺卜酯 /
- SO42-/ZrO2-TiO2 /
- 微波辐射 /
- 催化合成
Abstract:Nopyl acetate was synthesized by nopol and acetic acid under microwave irradiation and catalyzed by solid superacid SO42-/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.
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Keywords:
- nopyl acetate /
- SO42-/ZrO2-TiO2 /
- microwave irradiation /
- catalytic synthesis
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