论文总字数：25104字

摘 要

丙烯酸丁酯是一种十分重要的聚合物单体和有机合成中间体，其聚合物和共聚物在各个工业领域及日常生活中都有广泛的应用。固体酸催化剂在石油精炼和精细化工中占有重要地位，其在工业生产上应用广泛。生物质活性炭材料是一种新颖的材料，这种材料可以作为优良的催化剂载体，因为其具有较高的比表面积和孔体积、良好的物理化学性能、丰富的表面官能团。开发能够应用于精馏残液催化酯化的固体酸催化剂来减少其产生的废弃物具有重要的现实和研究意义。

论文以淀粉和正硅酸四乙酯为前驱体通过改变活化条件制备了一系列键连磺酸基团的固体酸催化剂。通过FT-IR、TG、BET等一系列实验手段对催化剂进行了表征。表征结果表明，催化剂表面平整均衡且存在孔结构，热稳定性良好，有键连磺酸基团存在。实验结果表明，在以KOH为活化剂，碱碳质量比为2，在800 ºC活化3小时等实验条件下，活性炭为负载体制备的催化剂具有最大的比表面积（1823.1 m²/g）和孔体积（0.77 cm³/g）。以正丁醇和丙烯酸的酯化反应作为探针反应，考察了活化方法、时间、温度、碱碳比等主要因素对催化剂性能的影响。为验证制备的催化剂的重复性，我们对其做了一些实验，实验结果表明，AC-700/180/2具有很好的重复性，在多次重复使用后催化效果仍然良好。

关键词: 活性炭 固体酸 催化 酯化

Preparation of starch-based activated carbon solid acid catalyst and its catalytic performance

Abstract

Butyl acrylate is a significant polymer monomer and organic synthesis intermediate, and its polymer and copolymer have been widely used in various industrial fields as well as daily life. Solid acid catalysts, which are widely used in industrial production, play an important role in petroleum refining and fine chemical industry. Biomass activated carbon material, which could be used as an excellent catalyst carrier, is a novel material for the reason that it has high specific surface area, pore volume, good physical and chemical properties and all kinds of surface functional groups. It is of great practical and research significance to develop solid acid catalysts for catalytic esterification of distillation residues.

In this thesis, using starch and tetraethyl orthosilicate as precursors, a series of solid acid catalysts bonded with sulfonic groups were produced by changing the activation conditions. The catalysts were characterized by FT-IR, TG, BET and other experimental methods. The characterization results proved that the surface of the catalyst was flat and balanced with pore structure, and has good thermal stability and shows the presence of bonded sulfonic acid groups. The experimental results confirmed that the catalyst loaded on activated carbon had the maximum specific surface area (1823.1 m²/g) and pore volume (0.77 cm³/g) under the experimental conditions of KOH as the activator, alkali carbon mass ratio (2) and activation at 800 ℃ for 3 hours. The influence of the activation method, time, temperature and alkali-carbon ratio on the performance of the catalyst was investigated by the esterification of n-butanol and acrylic acid as probe reaction. In order to verify the repeatability of the prepared catalyst, we conducted some more experiments on it. The experimental results showed that ac-700/180/2 had good repeatability, and the catalytic effect was still good after repeated use.

Keywords: activated carbon solid acid catalyze  esterification

目 录

摘 要 I

Abstract II

第一章 文献综述 1

1.1丙烯酸丁酯综述 1

1.1.1丙烯酸丁酯的应用 1

1.1.2 丙烯酸丁酯的合成 2

1.1.3用于制备丙烯酸正丁酯的催化剂研究进展 4

1.2生物质活性炭 4

1.2.1物理活化法 6

1.2.2化学活化法 6

1.2.3 活化剂 7

第二章 实验内容 10

2.1 前言 10

2.2 实验部分 10

2.2.1 实验药品及仪器 10

2.2.2以淀粉基活性炭为负载剂的催化剂的制作 12

2.2.3以商业活性炭为负载剂的催化剂的制作 13

2.2.4催化剂的催化性能评价 13

2.3实验结果与讨论 14

2.3.1测定催化剂中的酸 14

2.3.2红外谱图分析 15

2.3.3 催化剂热稳定性分析 16

2.3.4催化剂比表面积分析 16

2.4考察催化剂的性能 18

2.4.1活化催化剂的方法的影响 18

2.4.2温度的影响 19

2.4.3时间因素的影响 19

2.4.4碳碱比因素的影响 20

2.5 本章小结 20

第三章 总结与结论 22

参考文献 23

致 谢 28

第一章 文献综述

1.1丙烯酸丁酯综述

1.1.1丙烯酸丁酯的应用

丙烯酸丁酯，又称为丙烯酸正丁酯与2-丙烯酸丁酯，是一种无色透明液体，具有强烈刺鼻的芳香气味，分子式为C₇H₁₂O₂。化学类别为丙烯酰基化合物。毒性与丙烯酸甲酯相接近，对人体的皮肤和眼部具有比较大的刺激性。几乎不溶于液体水、无机溶剂，可溶于酮类、醇类、醚类、烃类等有机溶剂。丙烯酸丁酯在工业上是一种十分重要的聚合物单体和有机合成中间体，可以和苯乙烯、缩水甘油酯、丙烯腈、羟丙酯等单体共聚、接枝和交联。丙烯酸丁酯可广泛应用于涂料油漆、合成纤维、合成橡胶、塑料、皮革、纺织、压敏胶、造纸、粘合剂、包装材料、水处理、冶金采矿、日用化工产品等工业领域^[1-2]，尤其在做MBS以及MMA树脂改性剂时，在国外受到很多关注。

（1）涂料行业的应用

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