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作 者:卜佳[1] 李广学[1] 赵明珠[1] 李家鸣[1] 姜丰[1] 詹华露[1] 褚杨[1]
机构地区:[1]安徽理工大学化学工程学院,安徽淮南232001
出 处:《精细石油化工》2012年第5期51-54,共4页Speciality Petrochemicals
基 金:安徽省经信委-技术创新项目(2010-淮南-13)
摘 要:以环戊酮和正戊醛为起始原料,经羟醛缩合、选择性催化加氢、氧化重排制得δ-癸内酯。通过正交实验,得出最佳工艺条件:w(NaOH)=1%,PEG-600用量0.7g,草酸用量0.2g,n(双氧水)∶n(2-戊基环戊酮)=4∶1,甲醇用量30mL,硫酸用量2mL,反应收率为61.2%。采用红外光谱对产物结构进行了表征。A new method is presented for synthesizing δ-decalactone from n-valeraldehyde and cyclopentanone via the reaction process of aldol condensation,selective catalytic hydrogenation and oxidation.The optimum process conditions acquired through the orthogonal experiments were as follows: w(NaOH) = 1%,m(PEG-600)=0.7 g,m(oxalic acid)=0.2 g,n(hydrogen peroxide)∶n(2-amyl cyclopentanone)=4∶1,V(methanol)=30 mL,V(sulfuric acid)=2 mL,and the final yield was 61.2%,which is superior to the literature reported value of 52%.The intermediates and product were characterized by IR and GC-MS.To compare with the traditional methods,the raw materials are easy available,the reaction route is simple,the product yield is relatively high and the operation is quiet safe via this method.
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