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作 者:段练
机构地区:[1]中国石油化工股份有限公司齐鲁分公司研究院,山东淄博255400
出 处:《山东化工》2007年第3期5-8,共4页Shandong Chemical Industry
摘 要:以Koch反应合成三甲基乙酸。实验工艺中三甲基乙酸的收率(以异丁烯计)高达76.11%(平均值为73.17%),纯度高,实验重复性良好。小试确立了适宜的Koch反应合成条件:反应温度为30℃、反应压力为5.0MPa、硫酸与异丁烯的物质的量比为4.5、溶剂与异丁烯的质量比为3.5、反应时间为2h、进料时间为3h、异丁烯的进料量为1.0mol,n(异丁烯)∶n(溶剂)∶n(H2SO4)=1∶2.3∶4.5。三甲基乙酸的收率以异丁烯计可达77.19%以上,三甲基乙酸的纯度可达99.00%以上。水解反应的适宜条件为:水量为200.0g、水解时间为80m in、水解温度为20℃。To produce trimethylacetic acid with Koch reaction,in the experimental technological process,the yield(isobutene calculated)of trimethylacetic acid was increased to 76.11%(average value is 73.17%),the purity of trimethylacetic acid was high,and the repetition of experiments was perfect.The optimum reaction conditions were as follows: reaction temperature was 30℃,reaction pressure was 5.0MPa,the molar ratio of sulfuric acid to isobutylene was 4.5,the mass ratio of solvent to isobutylene was 3.5,reaction time was 2 h,the feeding time was 3h,the isobutylene feed was 1.0 mole,n(isobutene) ∶ n(solvent) ∶n(catalyst) = 1∶2.3∶4.5.The yield(isobutene calculated)of trimethylacetic acid was above 77.19% and the purity of trimethylacetic acid was above 99.00%.The optimum hydrolysis reaction conditions were as follows:the mass of water used in hydrolysis reaction was 200.0g,hydrolysis reaction temperature was 20℃,hydrolysis reaction time was 80min.
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