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机构地区:[1]上海华谊集团技术研究院,上海200241 [2]上海华谊丙烯酸有限公司,上海200137
出 处:《精细化工中间体》2011年第5期41-44,共4页Fine Chemical Intermediates
摘 要:以丙烯酸甲酯和环己醇为原料,经过酯交换反应合成γ,γ-环戊基丁内酯,γ,γ-环戊基丁内酯加氢得到3-环己基丙酸。考察了2步反应的催化剂和反应条件对产物收率的影响。研究结果表明,酯交换反应的优化条件为:过氧化二叔丁基为引发剂,n(丙烯酸甲酯)∶n(环己醇)=1∶4,反应温度160℃,反应时间6 h;在该条件下,γ,γ-环戊基丁内酯的收率可达93.3%;以0.5%铅/氧化铝为催化剂,γ,γ-环戊基丁内酯加氢反应的优化条件为:反应温度为250℃,γ,γ-环戊基丁内酯空速0.2 h-1,反应压力3.0 MPa,氢气空速500 h-1,在该条件下,γ,γ-环戊基丁内酯转化率78.0%,环己基丙酸选择性80.2%。3-Cyclohexylpropionic acid was prepared by hydrogenation ot y,y-cyclopentyl outyrolactone, which was synthesized by transesterification of methyl acrylate and cyclohexanol. The influences of catalyst and reaction conditions have been studied. The optimum conditions for the transesterification include the temperature of 160℃, the molar ratio of methyl acrylate to cyclohexanol of 1 to 4, the reaction time of 6 hours and di-tert-butyl peroxide as the initiator. Over the catalyst of 0.5%Pd/A1203, the conversion of T,T-cyclopentyl butyrolactone and the selectivity of 3-cyclohexylpropionic acid can reach 78.0% and 80.2%, respectively, under the optimum condition of 250℃, 3.0 MPa, LHSV of y,y-cyclopentyl butyrolactone of 0.2 h-1 and GHSV of H2 of 500 h-1.
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