碳基固体酸的制备及在丁二酸酯合成中的应用

摘要：本论文是以自然界中的天然原料核桃壳作为碳源，通过碳化、磺化等方法制备出了碳基磺酸型固体酸。并以在不同条件下制备出来的固体酸作为催化剂，通过催化丁二酸和正丁醇来酯化合成丁二酸二丁酯的反应来考察此类催化剂的催化性能。通过大量实验表明，当丁二酸的用量为0.06mol, n丁二酸：n正丁醇=1:3，催化剂的投料量为4g，催化反应时间为4h时，由核桃壳制备出的碳基磺酸型固体酸具有较好的催化活性。其最佳的制备工艺条件为：碳化时间3h、磺化时间4h、碳化温度80℃、磺化温度90℃、核桃壳与浓硫酸的质量比为1:10,以此条件下所制备得到的碳基磺酸型固体酸催化酯化合成丁二酸二丁酯的收率为82.3％。酯化产物的结构已经通过核磁共振光谱图进行了表征。35012
毕业论文关键词：碳基固体酸；酯化；丁二酸酯
Carbon based solid acid preparation and Application of ester succinate synthesis
Abstract： This paper is based on the natural raw materials of walnut shell as the carbon source, through carbonization and sulfonation were prepared by carbon based solid acid sulfonic acid. According to the different conditions of the preparation of solid acid as catalyst, catalyzed bysuccinic acid and n-butanol to synthesize ester succinate to examine the activity of the catalyst. Experiments show that, when the dosage is 0.06mol of succinic acid, n(succinic acid):n (n-butanol)=1:3, the amount of catalyst is 4g, the reaction time is 4h, the carbon based solid acidsulfonic acid walnut shell preparation has good catalytic activity, and the best preparation conditions were: the carbonization time is 3h, the sulfonation time is 4h, the carbonization temperature is 80 centigrade, the sulfonation temperature is 90 centigrade, carbide and sulfuric acid is 1:10. Carbon based solid acid catalytic esterification of sulfonic ester was prepared under the condition of succinic acid and the yield was 82.3%. The structure of product was characterized by infrared spectroscopy and nuclear magnetic resonance.
Key Words:Carbon based solid acid ; esterification; ester succinate
目录
1前言    1
1.1 开题依据    1
    1.2.固体酸催化剂概述    1
1.2.1固体酸催化剂简介    2
1.2.2固体酸催化剂分类    2
1.3丁二酸酯类的研究状况    4
1.4丁二酸二丁酯的合成方法    8
1.4.1催化酯化法    8
1.4.2酰卤法    9
1.4.3以丙烯酸酯为原料合成    9
2 实验部分    10
2.1仪器与试剂    10
2.1.1仪器    10
2.1.2试剂    10
2.2实验步骤    10
2.2.1碳基固体酸催化剂的制备    10
2.2.2 丁二酸二丁酯的合成    11
2.2.3实验装置    11
3结果与讨论    12
3.1碳化温度对产物产率的影响    12
3.2碳化时间对产物产率的影响    13
3.3磺化温度对产物产率的影响    14
3.4磺化时间对产物产率的影响    15
3.5壳与硫酸的质量比对产物产率的影响    16
4产物分析    18
4.1产物折射率分析    18
4.2核磁共振谱图分析    18
5结论    19
6致谢    20
参考文献    21
1 前言
1.1开题依据
丁二酸二丁酯，又名琥珀酸二丁酯,是一种重要的化工中间体，它目前主要应用于染料、医药、农产品加工和气相色谱固定液等领域。工业上较为常规的合成方法是在浓硫酸的催化作用下由丁二酸和正丁醇酯化反应而成。然而硫酸其本身具有强酸性、强腐蚀性，还易引起副反应的发生，如炭化、氧化和聚合反应等。同时，它对环境的污染也是当前化工生产行业中极需解决的问题。碳基固体酸的制备及在丁二酸酯合成中的应用:http://www.youerw.com/yixue/lunwen_32752.html