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1.2MPa下反应4 h,产物DOMA收率可达75.6%。
（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-butylammonium 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.
出处
《精细化工中间体》
CAS
2013年第1期51-54,72,共5页
Fine Chemical Intermediates
