摘要:本论文以竹子作为生物碳原,通过浓硫酸炭化、磺化制备竹碳基磺酸固体酸,以此为催化剂催化环己酮与乙二醇反应制备环己酮乙二醇缩酮来考察该固体酸催化剂的催化活性。
本毕业论文探讨了竹碳基磺酸固体酸制备中的炭化时间、磺化温度、磺化用酸的竹酸质量比、磺化时间的最佳工艺重要条件。实验表明,当n环己酮:n乙二醇=1:1.5,催化剂用量为总质量5%,炭化竹粉浓硫酸质量比为1:8,竹粉炭化温度80℃,炭化时间2.5h;磺化竹粉浓硫酸质量比为1:6,磺化温度80℃,磺化时间2h,环己酮乙二醇缩酮收率可达75.2%。通过红外光谱、核磁共振对产物环己酮乙二醇缩酮的结构进行表征。19869
关键词:生物碳基磺酸;竹;环己酮乙二醇缩酮;催化;
Synthesis of cyclohexanone ethylene ketal catalyzed by biomass char sulfonic acid
Abstract: In this paper, using bamboo as raw material, by concentrated sulfuric acid charring and sulfonated to prepare biomass char sulfonic acid. Synthesis of cyclohexanone ethylene ketal catalyzed by biomass char sulfonic acid to investigated the catalytic activity of the solid acid catalyst.
In this paper, preparation conditions were optimized about charring time, sulfonated temperature, mass ratio of Bamboo and acid in the sulfonation, sulfonated time. In the Ketalization Reactions, n Cyclohexanone:n ethylene glycol=1:1.5, 1.0g biomass char sulfonic acid as a catalyst, synthesis of cyclohexanone ethylene ketal by heated to watershed reflux for 1h. By yield of cyclohexanone ethylene ketal to verify catalytic ability of the biomass char sulfonic acid. The optimistical charring conditions are concentration of sulfuric acid being 98%,mass ratio of Bamboo and acid in the carbonization being 1:8,charring time being 2.5 h,and charring temperature being 80℃.The optimistical sulfonation conditions are concentration of sulfuric acid being 98%,mass ratio of Bamboo and acid in the sulfonation being 1:6,sulfonation time being 2 h,and sulfonation temperature being 80℃.Synthesis of cyclohexanone ethylene ketal catalyzed by bamboo char sulfonic acid prepared In this condition, yield of the crude product yield was 75.2%. To detect product by the refractive index and nuclear magnetic resonance spectroscopy.
Key words: biomass char sulfonic acid; bamboo; cyclohexanone ethylene ketal; catalyst; preparation
目录
1、前言 1
1.1开题依据 1
1.2固体酸简介 1
1.2.1固体酸分类 1
1.2.2固体酸的改性 3
1.2.3生物碳基类固体酸 4
1.3合成缩醛(酮)用固体酸的研究概况 5
1.4环己酮乙二醇缩酮的合成 6
1.5本论文的研究思路与研究内容 7
2 实验部分 9
2.1仪器与试剂 9
2.1.1仪器 9
2.1.2试剂 9
2.2实验步骤 10
2.2.1固体酸催化剂的制备 10
2.2.2环己酮乙二醇缩酮的制备 10
2.2.3实验装置 10
3结果与讨论 12
3.1炭化时间对催化剂催化能力的影响 12
3.2磺化温度对催化剂催化能力的影响 13
3.3竹酸质量比对催化剂催化能力的影响 14
3.4磺化时间对催化剂催化能力的影响 15
4产物分析 17
4.1折光率分析 17
4.2红外光谱分析 17
4.3核磁共振谱分析 18
5结论 20
6致谢 21
参考文献 22
1 前言
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