固体酸催化合成丙烯酸异冰片酯工艺条件优化

Process Optimization for Synthesis of Isobornyl Acrylate over Solid Acid Catalyst

以莰烯和丙烯酸为原料,在自制固体酸催化剂的作用下合成了丙烯酸异冰片酯,研究了反应条件对产品收率的影响。在单因素实验基础上,采用响应面分析法对合成工艺条件进行了优化。实验结果表明:各因素对丙烯酸异冰片酯收率影响从大到小依次为催化剂用量,酸烯比,反应时间和反应温度;得到较好的合成工艺条件为酸烯物质的量之比为1.3,催化剂用量为15.5%(相对莰烯的质量百分比),反应温度61℃,时间7.9 h。在此条件下产品收率为81.3%,利用气相色谱-质谱(GC/MS)与核磁共振(1H NMR)对丙烯酸异冰片酯产物进行分析,结果表明产物纯度很高。

The isobornyl acrylate was synthesized using camphene and crylic acid as raw materials over the self-made solid acid catalyst and the effect of reaction conditions on the yield of product was studied.On the basis of single-factor tests,the response surface methodology was used to optimize the reaction conditions.The results showed that the influence of each factor on the yield of isobornyl acrylate was in the order(from large to small)of catalyst dosage,molar ratio of acrylic acid to camphene,reaction time and reaction temperature.The optimized reaction conditions were as follows:the molar ratio of acrylic acid to camphene1.3,the mass fraction of catalyst15.5%(relative to the mass percentage of camphene),the reaction temperature61℃and reaction time7.9h.Under these optimized reaction conditions,the maximum yield of isobornyl acrylate was81.3%.The product of isobornyl acrylate was characterized by gas chromatography-mass spectrometer(GC-MS)and1H nuclear magnetic resonance(1H NMR).The results showed that the purity of isobornyl acrylate was high.