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作 者:张旭[1] 孙晋蒙 刚勇[1] 郭宏垚 李冬[1] 李稳宏[1]
机构地区:[1]西北大学化工学院
出 处:《精细化工》2018年第2期333-339,共7页Fine Chemicals
基 金:陕西省教育厅服务地方专项计划项目(14JF026)~~
摘 要:以1,4-丁二醇和丙烯酸为原料,采用制备的SO^2-4/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∶1.00,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%。通过核磁共振氢谱确认产品为BDDA,其各项理化指标均符合相关标准,液相色谱纯度为95%~98%,酸值为0.133 mg KOH/g,明显优于标准品。1 ,4-Dutanediol diacrylate (BDDA) was prepared from 1,4-butanediol and acrylic acid on SO42/TiOz-SnOz solid acid catalyst. The effects of molar ratio of acrylic acid to 1,4-butanediol, amount of catalyst,reaction temperature and reaction time on the conversion of 1,4-butanediol and the yield of 1,4-butanediol diacrylate were studied. Subsequently ,the process conditions for the synthesis of BDDA were optimized by response surface methodology on the basis of single-factor tests. The optimized process conditions were obtained as follows: the molar ratio of acrylic acid to 1,4-butanediol was 2.62 :1.00, the amount of catalyst was 8. 88% of the total mass of 1,4-butanediol and acrylic acid, the reaction temperature was 136.24 ℃ and reaction time was 4.68 h. Considering the actual situation, the reaction temperature was trimmed about 136 ℃. Meanwhile, five experiments were performed to test the repeatability of BDDA yield. The average yield of BDDA was 88.12%. Nuclear magnetic resonance (NMR) measurement results confirmed that the structure of the synthesized compound was consistent with that of 1,4-butanediol diacrylate. In addition, all physicochemical indexes of BDDA met relevant standards. Especially, the purity and acid value of BDDA were in the range between 95 % and 98% and 0. 133 mg KOH/g,respectively,which was obviously better than that of BDDA standard sample.
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