| 第 43 卷第 1 期 |  | Vol. 43 No. 1 | | 2013 年 2 月 | Feb 2013 |
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所属栏目：功能材料
利用二氧化碳和甲基丙烯酸缩水甘油酯制备环碳酸酯的研究 |
| 李祥龙1，李吉明1，闫占磊1，张晓林2
（1. 滨州市安全评价中心，山东 滨州 256600；2. 南昌大学 环境与化学工程学院，江西 南昌 330031） |
| 摘 要：以含有环氧基团和双键结构的甲基丙烯酸缩水甘油酯（GMA）与二氧化碳为原料合成用于制取新型环保材料非异氰酸酯聚氨酯的中间体环碳酸酯（DOMA），考察了催化剂、反应温度、压力、以及时间等反应条件对产物DOMA收率的影响，并对原料和产物通过TGA、红外进行分析，对产物通过碳谱、氢谱进行结构表征，表明在溶剂存在下，以四丁基溴化铵与碘化锌为共催化剂，在温度为110℃、压力为1.2 MPa下反应4 h，产物DOMA收率可达75.6%。 |
| 关键词：甲基丙烯酸缩水甘油酯；二氧化碳；环碳酸酯；非异氰酸酯聚氨酯 |
| 中图分类号：TQ430.4 文献标识码：A 文章编号：1009-9212（2013）01-0051-04 |
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| 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 |
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作者简介： 李祥龙（1984-），男，山东济宁人，硕士，研究方向：非异氰酸酯聚氨酯的合成、改性及应用。（E-mail：bename789@hotmail.com）
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收稿日期：2013-01-12
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