β-异佛尔酮合成的新工艺研究  

Study on New Process for the Synthesis of β-isophorone

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作  者:区家杰 叶振兴 林嘉玮 Ou Jiajie;Ye Zhenxing;Lin Jiawei(Guangzhou Juyuan Bio-chem Co.,Ltd.,Guangzhou 510000;Zhaoqing Juyuan Bio-chem Co.,Ltd.,Zhaoqing 526000,China)

机构地区:[1]广州巨元生化有限公司,广东广州510000 [2]肇庆巨元生化有限公司,广东肇庆526000

出  处:《广东化工》2021年第13期35-36,共2页Guangdong Chemical Industry

摘  要:以α-异佛尔酮为原料,通过缩酮反应、异构化及缩酮脱保护三步,再经过精馏得到β-异佛尔酮纯品。考察了催化剂、反应温度等对反应的影响,并对反应条件进行了优化。实验结果表明,使用对甲苯磺酸作为缩酮反应和异构化的催化剂,使用无水氯化铁作为脱保护催化剂,可得到含量大于50%的β-异佛尔酮混合物。该混合物在温度120℃,压力20 mbar条件下减压精馏,可得到含量大于98%的β-异佛尔酮。β-isophorone was obtained from α-isophorone through three steps of ketal reaction, isomerization and ketal deprotection, and then rectified. The effects of catalyst and reaction temperature on the reaction were investigated, and the reaction conditions were optimized. The results show that under the optimum conditions of using p-Ts OH as the ketal reaction and isomerization catalyst, and using anhydrous FeCl3 as the deprotection catalyst, a mixture of β-isophorone with a purity of more than 50 % can be obtained. The mixture is rectified at a temperature of 120 ℃ and a pressure of 20 mbar to obtain β-isophorone which purity can reach to 98 %.

关 键 词:异佛尔酮 缩酮反应 异构化 脱保护 催化剂 

分 类 号:TQ[化学工程]

 

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