離子液體用作甲苯二胺與乙烯烷基化催化劑的探索

摘要
　　　二乙基甲苯二胺（DETDA）是聚氨酯的擴(kuò)鏈劑，工業(yè)上一般采用無機(jī)AlCl3催化甲苯二胺（TDA）和乙烯烷基化反應(yīng)制得，但是該工藝過程在高溫高壓下操作，存在較大的安全隱患，設(shè)備腐蝕和污染嚴(yán)重。氯鋁酸類離子液體相對(duì)無機(jī)AlCl3催化劑，具有酸度分布均勻，酸性可調(diào)，環(huán)保安全的特點(diǎn)，理論上有更好的催化活性，能有效夠降的降低反應(yīng)溫度和壓力。本論文旨在采用酸性離子液體作為催化劑，探索開發(fā)烷基化制備DETDA的新技術(shù)。
　　　論文建立了色譜分析DETDA及TDA的檢測(cè)方法；考察了DETDA及TDA在甲苯、CH2Cl2等不同溶劑及離子液體中的溶解度；采用堿水破壞和溶劑萃取的方法對(duì)DETDA，TDA，離子液體三者的混合物進(jìn)行分離。結(jié)果表明首先采用NaOH溶液對(duì)離子液體進(jìn)行分解，再用CH2Cl2對(duì)溶液進(jìn)行萃取的分離效果最好。其DETDA的回收率可達(dá)89.70%，TDA的回收率可達(dá)72.87%。
　　　論文對(duì)離子液體催化TDA與乙烯的烷基化反應(yīng)條件進(jìn)行了初步探索，結(jié)果表明，在反應(yīng)溫度大于180 ℃，反應(yīng)壓力大于2 MPa的條件下，反應(yīng)能夠進(jìn)行。


關(guān)鍵詞：DETDA；離子液體；烷基化；萃取分離
　　　

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 錄
第1章 前言 1
第2章 文獻(xiàn)綜述 2
2.1 DETDA概述 2
　　2.1.1 DETDA與TDA的性質(zhì)及用途 2
　　2.1.2 DETDA的合成工藝及催化劑 3
　　2.1.3 DETDA的檢測(cè)方法 4
2.2 離子液體簡(jiǎn)介及應(yīng)用 5
　　2.2.1 離子液體概述 5
　　2.2.2 離子液體的應(yīng)用 7
2.3 文獻(xiàn)綜述小結(jié) 9
第3章 實(shí)驗(yàn)部分及討論 11
3.1 DETDA和TDA的色譜檢測(cè)方法 11
　　3.1.1 實(shí)驗(yàn)所用儀器 11
　　3.1.2 色譜操作條件 11
　　3.1.3 色譜圖像及分析 11
3.2 DETDA，TDA，IL的模擬分離 13
　　3.2.1 DETDA，TDA的溶解性能 13
　　3.2.2 DETDA與IL的分離性能 13
　　3.2.3 DETDA，TDA，IL三者模擬分離 14
3.3 TDA與乙烯合成DETDA的反應(yīng) 16
　　　3.3.1 實(shí)驗(yàn)所用儀器 16
　　3.3.2 合成反應(yīng)步驟 17
　　3.3.3 合成反應(yīng)實(shí)驗(yàn)結(jié)果 18
第4章 總結(jié) 19
參考文獻(xiàn) 錯(cuò)誤！未定義書簽。
致 謝 22