离子液体用作甲苯二胺与乙烯烷基化催化剂的探索.doc
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离子液体用作甲苯二胺与乙烯烷基化催化剂的探索,摘要 二乙基甲苯二胺（detda）是聚氨酯的扩链剂，工业上一般采用无机alcl3催化甲苯二胺（tda）和乙烯烷基化反应制得，但是该工艺过程在高温高压下操作，存在较大的安全隐患，设备腐蚀和污染严重。氯铝酸类离子液体相对无机alcl3催化剂，具有酸度分布均匀，酸性可调，环保安...
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离子液体用作甲苯二胺与乙烯烷基化催化剂的探索
摘要
二乙基甲苯二胺（DETDA）是聚氨酯的扩链剂，工业上一般采用无机AlCl3催化甲苯二胺（TDA）和乙烯烷基化反应制得，但是该工艺过程在高温高压下操作，存在较大的安全隐患，设备腐蚀和污染严重。氯铝酸类离子液体相对无机AlCl3催化剂，具有酸度分布均匀，酸性可调，环保安全的特点，理论上有更好的催化活性，能有效够降的降低反应温度和压力。本论文旨在采用酸性离子液体作为催化剂，探索开发烷基化制备DETDA的新技术。
论文建立了色谱分析DETDA及TDA的检测方法；考察了DETDA及TDA在甲苯、CH2Cl2等不同溶剂及离子液体中的溶解度；采用碱水破坏和溶剂萃取的方法对DETDA，TDA，离子液体三者的混合物进行分离。结果表明首先采用NaOH溶液对离子液体进行分解，再用CH2Cl2对溶液进行萃取的分离效果最好。其DETDA的回收率可达89.70%，TDA的回收率可达72.87%。
论文对离子液体催化TDA与乙烯的烷基化反应条件进行了初步探索，结果表明，在反应温度大于180 ℃，反应压力大于2 MPa的条件下，反应能够进行。
关键词：DETDA；离子液体；烷基化；萃取分离
Abstract
DETDA is an environmental protection chain extender. Traditionally, this kind of reaction take place in liquid phase catalyzed by AlCl3 use TDA with ethylene. But, the reaction take place in very high pressure and temperature, which cause a serious security problem as well as difficulties in recycling and disposal of the spent catalysts are drawbacks of these systems. In order to solve these problems, we want to use acidic ionic liquid as catalyst to design a new technology to complete this kind reaction .Alkylation of TDA with ethylene needs acidic liquid as catalyst, we use Et3NHCl/2AlCl3 ionic liquid in place of AlCl3, because that Et3NHCl/2AlCl3 is a strong aid. Another important reason is ionic liquid catalyze reaction more environmental protection and safe . Generally, ionic liquid catalyze reaction better than AlCl3 in theory., can reduce the reaction temperature and reaction pressure. We do research on using Et3NHCl/2AlCl3 ionic liquid as catalyst to design a new way to Synthesis DETDA.
We describe Chromatogram images of DETDA and TDA using the SP-3420 Chromatography and get the solubility of DETDA in solvents such as CH2Cl2, toluene. We use different reagents to separate mixture with DETDA,TDA ,IL and find that using NaOH could get the best effect of separation. We use NaOH to separate the mixture first, then , using CH2Cl2 as extractant could get good effect on separating the mixture The recovery of DETDA can reach 89.70% and the recovery of TDA can reach 72.87%。
With our research ,we get a conclusion that the reaction could take place in temperature higher than 180℃,pressure higher than 2MPa.
Key words: DETDA；ionic liquid；alkylation；extraction and separation
目 录
第1章 前言 1
第2章 文献综述 2
2.1 DETDA概述 2
2.1.1 DETDA与TDA的性质及用途 2
2.1.2 DETDA的合成工艺及催化剂 3
2.1.3 DETDA的检测方法 4
2.2 离子液体简介及应用 5
2.2.1 离子液体概述 5
2.2.2 离子液体的应用 7
2.3 文献综述小结 9
第3章 实验部分及讨论 11
3.1 DETDA和TDA的色谱检测方法 11
3.1.1 实验所用仪器 11
3.1.2 色谱操作条件 11
3.1.3 色谱图像及分析 11
3.2 DETDA，TDA，IL的模拟分离 13
3.2.1 DETDA，TDA的溶解性能 13
3.2.2 DETDA与IL的分离性能 13
3.2.3 DETDA，TDA，IL三者模拟分离 14
3.3 TDA与乙烯合成DETDA的反应 16
3.3.1 实验所用仪器 16
3.3.2 合成反应步骤 17
3.3.3 合成反应实验结果 18
第4章 总结 19
参考文献 错误！未定义书签。
致 谢 22
摘要
二乙基甲苯二胺（DETDA）是聚氨酯的扩链剂，工业上一般采用无机AlCl3催化甲苯二胺（TDA）和乙烯烷基化反应制得，但是该工艺过程在高温高压下操作，存在较大的安全隐患，设备腐蚀和污染严重。氯铝酸类离子液体相对无机AlCl3催化剂，具有酸度分布均匀，酸性可调，环保安全的特点，理论上有更好的催化活性，能有效够降的降低反应温度和压力。本论文旨在采用酸性离子液体作为催化剂，探索开发烷基化制备DETDA的新技术。
论文建立了色谱分析DETDA及TDA的检测方法；考察了DETDA及TDA在甲苯、CH2Cl2等不同溶剂及离子液体中的溶解度；采用碱水破坏和溶剂萃取的方法对DETDA，TDA，离子液体三者的混合物进行分离。结果表明首先采用NaOH溶液对离子液体进行分解，再用CH2Cl2对溶液进行萃取的分离效果最好。其DETDA的回收率可达89.70%，TDA的回收率可达72.87%。
论文对离子液体催化TDA与乙烯的烷基化反应条件进行了初步探索，结果表明，在反应温度大于180 ℃，反应压力大于2 MPa的条件下，反应能够进行。
关键词：DETDA；离子液体；烷基化；萃取分离
Abstract
DETDA is an environmental protection chain extender. Traditionally, this kind of reaction take place in liquid phase catalyzed by AlCl3 use TDA with ethylene. But, the reaction take place in very high pressure and temperature, which cause a serious security problem as well as difficulties in recycling and disposal of the spent catalysts are drawbacks of these systems. In order to solve these problems, we want to use acidic ionic liquid as catalyst to design a new technology to complete this kind reaction .Alkylation of TDA with ethylene needs acidic liquid as catalyst, we use Et3NHCl/2AlCl3 ionic liquid in place of AlCl3, because that Et3NHCl/2AlCl3 is a strong aid. Another important reason is ionic liquid catalyze reaction more environmental protection and safe . Generally, ionic liquid catalyze reaction better than AlCl3 in theory., can reduce the reaction temperature and reaction pressure. We do research on using Et3NHCl/2AlCl3 ionic liquid as catalyst to design a new way to Synthesis DETDA.
We describe Chromatogram images of DETDA and TDA using the SP-3420 Chromatography and get the solubility of DETDA in solvents such as CH2Cl2, toluene. We use different reagents to separate mixture with DETDA,TDA ,IL and find that using NaOH could get the best effect of separation. We use NaOH to separate the mixture first, then , using CH2Cl2 as extractant could get good effect on separating the mixture The recovery of DETDA can reach 89.70% and the recovery of TDA can reach 72.87%。
With our research ,we get a conclusion that the reaction could take place in temperature higher than 180℃,pressure higher than 2MPa.
Key words: DETDA；ionic liquid；alkylation；extraction and separation
目 录
第1章 前言 1
第2章 文献综述 2
2.1 DETDA概述 2
2.1.1 DETDA与TDA的性质及用途 2
2.1.2 DETDA的合成工艺及催化剂 3
2.1.3 DETDA的检测方法 4
2.2 离子液体简介及应用 5
2.2.1 离子液体概述 5
2.2.2 离子液体的应用 7
2.3 文献综述小结 9
第3章 实验部分及讨论 11
3.1 DETDA和TDA的色谱检测方法 11
3.1.1 实验所用仪器 11
3.1.2 色谱操作条件 11
3.1.3 色谱图像及分析 11
3.2 DETDA，TDA，IL的模拟分离 13
3.2.1 DETDA，TDA的溶解性能 13
3.2.2 DETDA与IL的分离性能 13
3.2.3 DETDA，TDA，IL三者模拟分离 14
3.3 TDA与乙烯合成DETDA的反应 16
3.3.1 实验所用仪器 16
3.3.2 合成反应步骤 17
3.3.3 合成反应实验结果 18
第4章 总结 19
参考文献 错误！未定义书签。
致 谢 22
