負(fù)載型n，n，n39;，n39;四甲基n”丙基胍及其離子液體的合成與表征

1、河北工業(yè)大學(xué)碩士學(xué)位論文負(fù)載型N，N，N'，N'-四甲基-N”-丙基胍及其離子液體的合成與表征姓名：鄭金穎申請學(xué)位級別：碩士專業(yè)：化學(xué)工藝指導(dǎo)教師：耿艷樓20080301負(fù)載型 N,N,N’,N’-四甲基-N’’-丙基胍及其離子液體的合成與表征 ii SYNTHESIS AND CHARACTERIZATION OF SILICA-SUPPORTED N,N,N’,N’- TETRAMETHYL -N’’- PROPYL

2、 GUANIDINE AND ITS IONIC LIQUID ABSTRACT Aminopropylated silica (APS), silica-supported N,N,N’,N’-tetramethyl-N’’-propyl guanidine (STMPG) and STMPG ionic liquids with different anions including PF6 -, CH3COO- and CF

3、3SO3 - were prepared. The structures of APS, STMPG and its ionic liquids were characterized by means of FTIR, BET, 13C MAS NMR, TG and elemental analysis. The different preparation methods were compared. APS was synthesi

4、zed separately by liquid-phase method and sol-gel method, and was characterized by means of FTIR, BET, elemental analysis and TG analysis. The surface of silica was pretreated via four kinds of methods to increase the qu

5、antity of hydroxyl group content and the result showed that microwave-activating was the most effective method: the number of hydroxyl group on the silica surface increased from 1.08 /nm2 to 1.29 /nm2. The loading of ami

6、nopropyl in the APS synthesized via liquid-phase method was 8.59wt%, the functional group concentration of aminopropyl was 1.49mmol/g and the pKa of APS was 9.3-15.0. The effects of some parameters on the sol-gel process

7、 were investigated and the optimal conditions were as follows: tetraethylorthosilicate(TEOS)/H2O=1/7 (molar ratio), TEOS/EtOH(ethanol)=1/6(molar ratio), aminopropyltriethoxysilane(APTES)/ TEOS=0.07 (mass ratio), T=35℃, p

8、H=9, aging time 72h. APS was extracted with dichloromethane for 4 h and dried at 393 K in vacuum for 6h. The loading and functional group concentration of aminopropyl in the APS synthesized via sol-gel method was 6.88wt%

9、 and 1.19mmol/g, respectively. The pKa of APS was 4.8, lower than that of APS synthesized via liquid-phase method. STMPG was prepared through three different methods. One synthetic method started with APS and tetramethyl

10、urea(TMU) in the presence of phosphorus oxy chloride (POCl3). The other two methods started with chloropropyltriethoxysilane (CPTES) and N,N,N',N'-tetramethy lguanidine (TMG). The structure of STMPG was character