丙酮缩二乙醇的合成工艺的研究毕业论文_化学工程与工艺毕业论文

丙酮缩二乙醇的合成工艺的研究毕业论文

2021-04-27更新

摘 要

2-乙氧基丙烯目前在国内已经逐步取代2-甲氧基丙烯成为合成克拉霉素的关键中间体,其合成方法通常采用两步法:1)以对甲苯磺酸为催化剂,无水乙醇为溶剂,采用原甲酸三乙酯与丙酮缩合制得丙酮缩二乙醇。2)以苯基甲基硅酸等为液相介质,对丙酮缩二乙醇进行高温(210℃)液相裂解,或以固体催化剂进行高温(160℃)气相裂解,可得到2-乙氧基丙烯。

本文主要探究2-乙氧基丙烯的合成工艺。以98%浓硫酸为催化剂,以原甲酸三乙酯和丙酮为反应原料,在不同恒温环境下的合成反应。探究不同时间点时产物的产率及副产物的含量。

实验结果表明:1)当催化剂含量高于0.06%后,决定反应进程的主要因素为温度,此时产物2-乙氧基丙烯的含量随温度升高而降低。

2)丙酮和甲酸乙酯的含量一直在28%左右波动起伏。

3)当催化剂含量在0.06%以下时,随温度的升高,2,2-二乙氧基丙烷的含量总体上是下降的;当催化剂含量在0.06%以上时,随温度的升高,2,2-二乙氧基丙烷的含量总体上是上升的。

4)在催化剂含量高于0.06%时,乙醇的含量随温度的升高而逐渐降低。

5)当催化剂含量高于0.09%,温度低于20℃时,原料原甲酸三乙酯基本反应完全;而当温度高于20℃时,原甲酸三乙酯有大量剩余。

关键词:2-乙氧基丙烯 98%浓硫酸 原甲酸三乙酯

Abstract

2 – Methoxypropene currently in the country has been gradually substituted by 2 – Ethoxypropene become a key intermediate in the synthesis of clarithromycin, which is usually made by a two-step synthesis method: 1) p-toluenesulfonic acid as a catalyst, ethanol as solvent, ethyl orthoformate acetone and acetone condensation system Diakylacetals. 2) as the liquid silicic acid phenylmethyl medium, acetone diethylacetal high temperature (210 ℃) liquid phase pyrolysis, the solid catalyst or a high temperature (160 ℃) gas-phase pyrolysis, to obtain 2 – ethoxy-propylene.

This paper explored 2 – Ethoxypropene synthetic process. 98% concentrated sulfuric acid as catalyst, triethyl orthoformate and acetone as raw materials, the synthesis reaction at different constant environment. Content and yield by products explore different points in time.

The results showed that: 1) when the content of the catalyst is higher than 0.06%, the main factors for the course of the reaction temperature, then the product, 2 – ethoxy content of propylene decreases with increasing temperature.

  1. The content of acetone and ethyl formate has been fluctuating at around 28 percent.
  2. When the catalyst content of 0.06% or less, with increasing temperature, 2,2 – diethoxy propane content is generally declining; When the catalyst content of 0.06%, the rise of temperature, 2 2 – diethoxy propane content is generally rising.
  3. When the content of the catalyst is higher than 0.06%, the content of ethanol with the temperature gradually decreased.

5) When the catalyst was higher than 0.09%, the temperature is below 20 ℃, the basic raw material triethyl orthoformate reaction is complete; and when the temperature is above 20 ℃, triethyl orthoformate a large surplus.

Keywords: 2-ethoxy propylene 98%Concentrated sulfuric acid Triethyl orthoformate

目录

1 绪论…………………………………………………………………………………………………………5

1.1 研究背景及意义……………………………………………………………………………………5

1.2 克拉霉素概述………………………………………………………………………………………5

1.2.1 克拉霉素的特性…………………………………………………………………………………5

1.2.2 克拉霉素研制的背景……………………………………………………………………………6

1.2.3 克拉霉素的研制…………………………………………………………………………………6

1.3 2-乙氧基丙烯………………………………………………………………………………………7

1.3.1 2-乙氧基丙烯的特性……………………………………………………………………………7

1.3.2 2-乙氧基丙烯的合成……………………………………………………………………………8

2 实验部分……………………………………………………………………………………………………9

2.1 实验仪器及原料……………………………………………………………………………………9

2.1.1 实验试剂……………………………………………………………………………………9

2.1.2 实验仪器……………………………………………………………………………………9

2.2 实验操作……………………………………………………………………………………………9

2.2.1 实验步骤……………………………………………………………………………………9

3 结果与讨论………………………………………………………………………………………………11

3.1实验分析……………………………………………………………………………………………11

3.2 实验数据表格………………………………………………………………………………………11

3.2.1 -10℃恒温环境下的反应情况……………………………………………………………11

3.2.2 0℃恒温环境下的反应情况………………………………………………………………14

3.2.3 10℃恒温环境下的反应情况………………………………………………………………16

3.2.4 20℃恒温环境下的反应情况………………………………………………………………19

3.2.5 30℃恒温环境下的反应情况………………………………………………………………21

3.2.6 小结…………………………………………………………………………………………24

3.3 结 论……………………………………………………………………………………………………26

致谢……………………………………………………………………………………………………………27

参考文献………………………………………………………………………………………………………28

1 绪论

1.1 研究背景及意义

2-乙氧基丙烯(英文名2-Ethoxypropene,分子式C5H10O),为无色透明且具有特殊气味的液体,不溶于水,与酮、醇等多种有机溶剂互溶,沸点62~64℃,是一种重要的医药中间体,目前在国内已经逐步取代2-甲氧基丙烯成为合成克拉霉素的关键中间体,合成方法通常采用两步法:1)以对甲苯磺酸为催化剂,无水乙醇为溶剂,采用原甲酸三乙酯与丙酮缩合制得丙酮缩二乙醇。

2)以苯基甲基硅酸等为液相介质,对丙酮缩二乙醇进行高温(210℃)液相裂解,或以固体催化剂进行高温(160℃)气相裂解,可得到2-乙氧基丙烯。反应原理如下:

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