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(完整版)氨基甲酸甲酯的合成与工艺优化毕业设计

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氨基甲酸甲酯的合成与工艺优化

Synthesis and process optimization of methyl

crbamate

目录

摘要 .............................................................................................................................. I Abstract ..................................................................................................................... II 引 言 .......................................................................................................................... 1 第一章 文献综述..................................................................................................... 2

1.1 酯类化合物简介............................................................................................. 2 1.2 氨基甲酸酯类化合物的应用 ........................................................................ 2 1.2.1 农药 .............................................................................................................. 2 1.2.2 医药 .............................................................................................................. 3 1.2.3 纺织行业 ...................................................................................................... 4 1.2.4 合成树脂改性.............................................................................................. 4 1.2.5 有机合成中间体.......................................................................................... 5 1.3 氨基甲酸甲酯的合成方法及研究现状 ........................................................ 6 1.3.1 光气法 .......................................................................................................... 6

1.3.2 有机碳酸酯胺解法...................................................................................... 6 1.3.3 羰基化法 ...................................................................................................... 8 1.3.4 尿素醇解法 ................................................................................................ 10 1.4 耦合反应 ....................................................................................................... 11 1.5 本课题的研究意义及主要内容 .................................................................. 12 1.5.1 本文研究内容............................................................................................ 13

第二章 实验部分................................................................................................... 14

2.1 氨基甲酸甲酯的合成................................................................................... 14 2.1.1 氨基甲酸甲酯的合成机理 ....................................................................... 14 2.1.2 实验试剂及仪器........................................................................................ 14 2.1.3 实验步骤 .................................................................................................... 15

第三章 实验结果和数据分析 ........................................................................... 16

3.1 图谱分析 ....................................................................................................... 16 3.1.1 热重分析 .................................................................................................... 16 3.1.2 红外光谱分析............................................................................................ 16 3.2 MC产率的计算 ............................................................................................ 18 3.3 实验条件的影响........................................................................................... 18 3.3.1 温度的影响 ................................................................................................ 18 3.3.2 压力的影响 ................................................................................................ 19 3.3.3 耦合剂用量的影响.................................................................................... 21

结论 ............................................................................................................................ 23 致谢 ............................................................................................................................ 24

参考文献 ................................................................................................................... 25

氨基甲酸甲酯的合成与工艺优化

摘要:本文综述了氨基甲酸酯类化合物在有机合成过程中作为中间体的主要用途,以及在农业、建筑、纺织等行业的应用。并对目前合成氨基甲酸酯的各种方法进行了评述。本文重点研究了氨基甲酸甲酯的合成路线,本文选择、安装了一套适用于高温、高压条件的带有电动搅拌装置、及精确控温、测温、测压器件的反应装置分别对用来测温测压力的热电偶和压力传感器进行了标定校正。选用了一套通过控制单一变量的分析方法,用于实验在不同反应条件下的最佳产率分析。通过大量试验分别考察了反应温度、反应压力、反应时间、耦合剂用量等因素对反应产率的影响,找到了此反应最适宜的温度、压力、反应时间和耦合剂用量。

关键词:氨基甲酸甲酯;多聚磷酸;尿素醇解法;耦合反应

Synthesis and process optimization of methyl carbamate

Abstract:The applications of methyl carbamate(MC) as intermediates in

the process of organic synthesis are reviewed in this paper. Methyl carbamate can also be used in agriculture, architecture, textile and so on. The different synthetic methods of methyl carbamate are also assessed. Preparation of methyl carbamate is the main content for this paper. A set of high-temperature and high-pressure resistant, stainless steel autoclave reactor is selected and installed. During the reaction process, the autoclave is electric-heated and electric-mixer. The temperature and pressure are detected and controlled respectively by thermocouple and pressure sensor, which have been precisely calibrated. In orner to analyze the experimental optimum yield under different reaction conditions, choosen a analysis of control method of single variable Experiments been carried out at different temperatures, pressures and coupling agent quantities for different time so as to acquire their effects on the synthesis reaction and to find the optimal reaction condition.

Keywords: Methyl carbamate; Polyphosphoric acid; Urea alcoholysis;

Coupling reaction;

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