固体酸法合成1,4-丁二醇二丙烯酸酯的工艺优化

Synthesis of 1,4-Butanediol Acrylate Process by Solid Acid

摘要:

以1,4-丁二醇和丙烯酸为实验对象，采用制备的SO42-/TiO2-SnO2作为固体酸催化剂合成1,4-丁二醇二丙烯酸酯（BDDA）。考察了酸醇物质的量比、催化剂用量、反应温度和反应时间对1,4-丁二醇转化率和BDDA产率的影响。在单因素实验的基础上，采用响应面分析法对BDDA的合成工艺进行了优化。优化的工艺条件为：酸醇物质的量比2.62:1，催化剂用量为1,4-丁二醇和丙烯酸总质量的8.88%，反应温度136.24℃，反应时间4.68h。考虑实际情况微调反应温度为136℃左右，进行5组重复性验证实验，得到BDDA的平均产率为88.12%。通过核磁共振分析确认产品为BDDA，各项理化指标均符合相关标准，其中液相色谱纯度为95%~98%，酸值为0.133 mgKOH/g，明显优于标准品。

Abstract:

SO42-/TiO2-SnO2 as solid acid catalyst was used for the synthesis of 1,4-butanediol acrylate with 1,4- butanediol and acrylic acid as experimental material. The effects of the mole ratio of acid to alcohol, the amount of catalyst, reaction temperature and reaction time on the conversion of 1,4- butanediol and yield of 1,4-butanediol acrylate were studied. The optimized process conditions were obtained by using response surface methodology on the based of single-factor tests. The optimized process conditions were as follow : the mole ratio of acid to alcohol of 2.62:1, the amount of catalyst of 8.88% of the total mass of 1,4- butanediol and acrylic acid, reaction temperature of 136.24℃ and reaction time of 4.68h. Considering the actual situation, the reaction temperature was trimmed about 136℃. Meanwhile, 5 groups of repeated verification experiments were carried and the average yield of 1,4-butanediol acrylate was 88.12%. By the NMR analysis confirmed that the products were 1,4-butanediol acrylate and the physicochemical indexes accord with relevant standards, especially the purity in 95%~98% and the acid value was 0.133 mgKOH/g. This was obviously better than the standards.