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作 者:赵德华[1] 陆向红[1] 计建炳[1] 计才千 张红红[3] 杨启炜[4] 郭少聪[4]
机构地区:[1]浙江工业大学浙江省生物燃料利用技术研究重点实验室,浙江杭州310014 [2]浙江工业大学化学工程学院,浙江杭州310014 [3]滨州学院化学工程系,山东滨州256600 [4]浙江大学生物质化学工程教育部重点实验室,浙江杭州310014
出 处:《化学工程》2017年第5期38-41,45,共5页Chemical Engineering(China)
摘 要:由于2,3,6-三甲基苯酚与其同系物的理化性质十分接近,高纯度2,3,6-三甲基苯酚的获取十分困难。文中采用COSMO-RS计算快速预筛选分离溶剂并初步探讨了分离机理。由计算结果可知:二甲基亚砜、甲醇、乙腈等氢键受体溶剂的选择性分配能力较高,且甲基酚主要依靠其极性及与溶剂的氢键作用的差异实现分离,与后续实验结果相符并减少了实验工作量。以乙腈为洗涤溶剂,用量为0.250 8 g/g原料,在20℃下,经单级固液萃取洗涤,固相产品中2,3,6-三甲基苯酚的质量分数由原料中的97.51%提高到98.49%,2,3,6-三甲基苯酚的收率为71.14%。多级固液萃取洗涤中,随着洗涤级数的增加,两相产品的纯度逐渐升高,而固相产品的总收率逐渐降低。Abstract :Pure 2,3,6-trimethyl phenol is hardly acquired because of the similar nature of methyl phenols. COSMORS calculation was applied for fast solvent screening and preliminary separation mechanism exploration. The eailculation results show that hydrogen bond aeeeptor solvents, including DMSO, methanol and aeetonitrile, owned high selective distribution capacity and the separation are mainly attributed to the difference of the polarity of methyl phenols and their hydrogen-bond interaction with solvents. The calaculation results are in good accordance with the experiment data. Meanwhile, the experiment workload was reduced by pre-screening of solvents through COSMO-RS calculation. When acetonitrile was used as the washing solvent with a consumption of 0. 250 8 g/g raw material, the mass fraction of 2,3,6-trimethyl phenol in solid phase product increased from 97.51% to 98.49% with a yield of 71.14% in single stage solid-liquid washing. In the multistage operation, the purity of two products increased with the washing stages, while the overall yield of solid product decreased simultaneously.
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