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催化合成水杨酸正戊酯的研究

论文编号:HG185 论文字数:9079,页数:23

摘 要: 本论文用正交试验法对常规加热合成水杨酸正戊酯和微波辐射合成水杨酸正戊酯进行了研究,并且通过实验数据分析得出了各自的最优条件。常规加热条件下,考察了醇酸比,搅拌速率,反应时间,催化剂用量四个因素对产率的影响,通过L16(44)正交实验和直观分析得出的最佳反应条件为:醇酸比为5:1,搅拌速率为300r/min, 催化剂用量为1.6ml,反应时间为4h,该条件下的酯化产率为76.40%。微波辐射条件下,考察了醇酸比,催化剂用量,反应温度,反应时间四个因素对产率的影响,通过L16(44)正交实验和直观分析得出的最佳反应条件为: 醇酸比为3:1,催化剂用量为1.1mL , 反应温度120℃,反应时间为40min。该条件下的酯化产率为84.79%。通过比较发现,把微波辐射技术应用于催化酯化反应,可以使反应时间缩短,产率增大。

关键词:水杨酸正戊酯;微波辐射合成;催化酯化;正交设计

Abstract: In this paper, we have used the orthogonal testing method to conventional method as well as the microwave radiation synthesis of amyl salicylate. then has worked out the optimized condition with intuitive analysis. In the conventional method, we have research different proportion of pentanol and salicylic acid, different mix blend velocity, different quantity of Sulfuric acid volume and different reaction time as four factors. Using L16 (44) orthogonal test and intuitive analysis ,the result enunciate that the most suitable and proper reaction conditions is that: the proportion of pentanol and salicylic acid is 5:1,mix blend the velocity is 300r/min, the Sulfuric acid volume is 1.6 mL, and reaction time is 4 hours, and the ester produces a rate of 76.40%. Then we complete synthesis of amyl salicylate at microwave radiation. It investigated the yield of ester by using different proportion of pentanol and salicylic acid, different quantity of sulfuric acid volume, different reaction temperature ,different reaction time . Using L16 (44) orthogonal test and intuitive analysis, the result enunciate that the most suitable and proper reaction conditions is that: the proportion of pentanol and salicylic acid is 3:1, the Sulfuric acid volume is 1.1 mL, reaction temperature 120℃,reaction time is 40 min, then the ester produces a rate of 84.79%. By comparison, the result shows that when microwave radiation technology was used in esterification, we can get short reaction times and high yields.

Keywords: Amyl salicylate; Microwave radiation; Catalytic esterification; Orthogonal design.

目 录

中文摘要I

英文摘要II

目录III

1. 绪论1

1.1 前言1

1.2 研究现状2

1.3 前景展望4

2. 实验部分5

2.1 实验原料与仪器5

2.1.1 实验原料 5

2.1.2 实验仪器 5

2.2 实验5

2.2.1 实验方案 5

2.2.2 产品分析 6

3. 结果与讨论7

3.1 常规加热合成水杨酸正戊酯的最优化设计7

3.1.1 正交试验方案设计7

3.1.2 实验结果与数据处理8

3.2 微波辐射合成水杨酸正戊酯的最优化设计10

3.2.1 单因素实验10

3.2.2 正交试验方案设计13

3.2.3 实验结果与数据处理14

4.总结与展望16

致谢18

参考文献19

附录21

催化合成水杨酸正戊酯的研究......