论文总字数：14062字

摘 要

柠檬酸酯类作为无毒增塑剂能用于生产包装材料和人体接触的医疗卫生用品等，在柠檬酸酯类无毒增塑剂中，目前已用于工业生产的是柠檬酸三丁酯（TBC）。柠檬酸酯系列增塑剂是一种绿色环保的新型增塑剂, 成为传统增塑剂邻苯二甲酸二辛酯(DOP) 的绿色替代品, 受到了广泛关注。

柠檬酸三丁酯传统的合成催化剂多是浓硫酸，但使用浓硫酸副反应多，污染环境并严重腐蚀设备，反应时间长、产品纯度低、后处理过程复杂。为此更换酯化催化剂已成为当今研究开发的热点．人们在探索新的催化剂。目前，合成TBC的新型催化剂主要有杂多酸、离子液体以及固体超强酸等为催化剂代替浓硫酸对这一反应的研究。本文主要讲使用活性炭负载钨硅酸作催化剂催化柠檬酸与正丁醇酯化合成柠檬酸三丁酯，并取得很好的酯化效果，研究表明：该反应具有催化剂用量少、催化剂易回收并可重复利用，反应速率快、产率较高等特点。

以活性炭负载硅钨酸为例，用活性炭负载硅钨酸催化剂催化柠檬酸与正丁醇酯化合成柠檬酸三丁酯。对柠檬酸与正丁醇酯化反应条件进行优化，其优化条件是：在酸醇的摩尔比为1:6，催化剂的负载量为17.9%，催化剂用量为柠檬酸质量的1.2%，反应温度为150℃，反应时间为4小时，柠檬酸的酯化率达92.3%，活性炭负载硅钨酸的收率为91.8%，产物经过红外光谱表征。

关键词：柠檬酸三丁酯；合成；硅钨酸；酯化

ABSTRACT

Citric acid esters can be used as a non-toxic plasticizer production of packaging materials and human contact, such as medical supplies, citric acid esters of non-toxic plasticizer, has been used for industrial production of citric acid tributyl (TBC). Citric acid ester series plasticizer is a new green plasticizer, a tradition octyl phthalate plasticizer (DOP) of green alternatives, received widespread attention.

Synthesis of tributyl citrate esters traditional catalyst is more concentrated sulfuric acid, but use the side reaction of sulfuric acid, environmental pollution and serious corrosion of equipment, long reaction time, the bottom of the product purity, complicated post-treatment process. To replace the esterification catalyst has become a hot spot in today's research and development. People in exploring new catalyst . Reportedly has a solid chloride , ion exchange resin, zeolite, heteropoly acid as catalyst instead of concentrated sulfuric acid such as the study of the reaction. This article mainly speak using tungstosilicic acid as a catalyst for catalytic activated carbon load of citric acid and n-butyl alcohol ester synthesis of tributyl citrate esters, and achieved good effect of esterification, research has shown that the reaction has the advantages of low dosage of catalyst, catalyst is easy to recycle and reuse, fast reaction rate and the characteristics of high yield.

Supported silicotungstic acid catalyst for the synthesis of citrate citric acid and butanol acid butyl ester three with active carbon. The citric acid and n-butyl alcohol esterification reaction conditions were optimized, the optimized conditions were: molar ratio of alcohol to acid 1:6.0, catalyst loading was 18%, the dosage of catalyst is 1.2% of the mass of citric acid, reaction temperature 150 ℃, reaction time 4 hours, the esterification of citric acid was up to 92.3%, the product through the infrared spectroscopic characterization.

KEYWORDS: Tributyl citrate；Synthesis；Silicotungstic acid；Esterification

目 录

摘要 2

ABSTRACT 3

目 录 5

第一章 文献综述 1

第二章 固体酸催化合成柠檬酸三丁酯的研究 7

2.1 主要试剂与仪器 7

2.2 实验部分 7

2.2.1 负载催化剂的制备 7

2.2.2 柠檬酸三丁酯的制备 7

第三章 结果和讨论 9

3.1 催化剂负载量对酯化反应的影响 9

3.2 反应时间对酯化率的影响 9

3.3 反应温度对酯化率的影响 10

3.4 酸醇摩尔比对酯化率的影响 10

3.5 催化剂重复使用对酯化率的影响 10

3.6 本章小结 11

第四章 结论 12

第五章 展望 13

参考文献 14

致 谢 17

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