| 第 43 卷第 1 期 |  | Vol. 43 No. 1 | | 2013 年 2 月 | Feb 2013 |
|
所屬欄目：功能材料
利用二氧化碳和甲基丙烯酸縮水甘油酯制備環(huán)碳酸酯的研究 |
| 李祥龍1，李吉明1，閆占磊1，張曉林2
（1. 濱州市安全評價(jià)中心，山東 濱州 256600；2. 南昌大學(xué) 環(huán)境與化學(xué)工程學(xué)院，江西 南昌 330031） |
| 摘 要：以含有環(huán)氧基團和雙鍵結構的甲基丙烯酸縮水甘油酯（GMA）與二氧化碳為原料合成用于制取新型環(huán)保材料非異氰酸酯聚氨酯的中間體環(huán)碳酸酯（DOMA），考察了催化劑、反應溫度、壓力、以及時(shí)間等反應條件對產(chǎn)物DOMA收率的影響，并對原料和產(chǎn)物通過(guò)TGA、紅外進(jìn)行分析，對產(chǎn)物通過(guò)碳譜、氫譜進(jìn)行結構表征，表明在溶劑存在下，以四丁基溴化銨與碘化鋅為共催化劑，在溫度為110℃、壓力為1.2 MPa下反應4 h，產(chǎn)物DOMA收率可達75.6%。 |
| 關(guān)鍵詞：甲基丙烯酸縮水甘油酯；二氧化碳；環(huán)碳酸酯；非異氰酸酯聚氨酯 |
| 中圖分類(lèi)號：TQ430.4 文獻標識碼：A 文章編號：1009-9212（2013）01-0051-04 |
|
| Synthesis of Cyclic Carbonate-DOMA with CO2 and GMA |
| LI Xiang-long1，LI Ji-ming1，YAN Zhan-lei1，ZHANG Xiao-lin2
（1. Binzhou Safety Assessment Center，Binzhou 256600，2. Department of Chemical Engineering，Nanchang University，Nanchang 330031，China） |
| Abstract：（2-oxo-1，3-dioxolan-4-yl）Methyl 2-methylprop-2-enoate（DOMA），which has cyclic carbonate structure and double bond structure，was synthesized from glycidyl methacrylate（GMA）and carbon dioxide as the raw materials in the presence of the solvent and catalyst under high pressure and high temperature. In order to improve the yield of DOMA，the effects of factors were discussed such as catalyst，temperature，pressure，and time. Crude product was obtained by means of washing，extraction and vacuum distillation，and the higher purity quotient of DOMA was refined by means of thin-layer chromatography and column chromatography，and the yield of DOMA content was examined by high performance liquid chromatography（HPLC）analysis. Experiments showed that the yield of DOMA was up to 75.6% on the condition that the catalyst was tetra-butyl-ammonium bromide（TBAB）and ZnI2，reaction temperature was 110℃，reaction pressure was 1.2 MPa，and the reaction time was 4 hours. The product after the reaction had been characterized by means of Fourier transform infrared spectroscopy（FTIR），Nuclear magnetic resonance spectroscopy carbon spectrum（13C-NMR，100 MHz，CDCl3），Nuclear magnetic resonance spectroscopy hydrogen spectrum（1H NMR，400 MHz，CDCl3），and the results proved that the functional groups and structure of the product were in accordance with DOMA. |
| Key words：glycidyl methacrylate；carbon dioxide；cyclic carbonate ester；NIPU |
|
作者簡(jiǎn)介： 李祥龍（1984-），男，山東濟寧人，碩士，研究方向：非異氰酸酯聚氨酯的合成、改性及應用。（E-mail：bename789@hotmail.com）
|
收稿日期：2013-01-12
|
|