环己醇残液中二环己基醚提取工艺及表征  

Extraction process and characterization of dicyclohexyl ether from cyclohexanol residue

作　　者：程伟琴 李迎春 鲁鹏 赵东璞[1,2] 王柏楠 霍二福 王宏力 CHENG Wei-qin;LI Ying-chun;LU Peng;ZHAO Dong-pu;WANG Bai-nan;HUO Er-fu;WANG Hong-li(Henan Chemical Industry Research Institute Co.,Ltd.,Zhengzhou 450052,China;Henan Engineering Research Center for Catalysis and Separation of Cyclohexanol,Zhengzhou 450001,China;Pingdingshan Shenma Wanli Chemical Company Limited,Pingdingshan 467000,China;Quality Inspection and Analytical Test Research Center,Henan Academy of Sciences,Zhengzhou 450008,China)

机构地区：[1]河南省化工研究所有限责任公司,河南郑州450052 [2]河南省环己醇催化分离工程研究中心,河南郑州450001 [3]平顶山市神马万里化工股份有限公司,河南平顶山467000 [4]河南省科学院质量检验与分析测试研究中心,河南郑州450008

出　　处：《现代化工》2021年第11期192-196,共5页Modern Chemical Industry

基　　金：河南省科学院基本科研业务费项目(190608026,200608012)。

摘　　要：通过两段空腔式玻璃弹簧填料精馏塔,采用减压精馏分离工艺提取环己醇残液中高附加值的二环己基醚。通过单因素实验探讨了真空度、回流比对二环己基醚提取效率的影响,获得了最佳的提取工艺条件:真空度为250 Pa、回流比为3∶1、精馏釜温度为125~135℃;经提取分离得到质量分数95%以上的二环己基醚,提取率为68.57%;质量分数为90%~95%的二环己基醚提取率为25.33%。通过气相色谱-质谱联用仪对环己醇残液、提取的二环己基醚及提取二环己基醚后的塔釜残液进行检测分析,结果表明,环己醇精馏残液主要成分为二环己基醚(84.33%,沸点242.5℃)、3-环己基环己烯(4.80%,沸点230.4℃)、1-环己基环己烯(5.29%,沸点234.2℃)和环己亚基环己烷(5.58%,沸点237.6℃);提取的二环己基醚质量分数最高可达99.80%,二环己基醚的总提取率为93.90%;精馏提取二环己基醚后,塔釜残液的主要成分为二环己基醚(86.30%)和1,1’-二羟基双环己基(13.70%)。High-value dicyclohexyl ether is extracted from cyclohexanol residue by vacuum distillation process in a two-section cavity glass spring packings distillation column.The effect of vacuum degree and reflux ratio on the extraction efficiency of dicyclohexyl ether is studied through single factor experiment.The optimum extraction conditions are obtained as follows:vacuum degree is 250 Pa,reflux ratio is 3∶1,and the temperature for rectifying kettle is in the range of 125-135℃.Under the optimal conditions,the extraction rate of dicyclohexyl ether with a purity of above 95%reaches68.57%,and the extraction yield of dicyclohexyl ether with a purity of 90%-95%is 25.33%.Gas chromatography/mass spectrometry(GC-MS)is employed to detect cyclohexanol residue,the extracted dicyclohexyl ether and tower kettle residue after extraction.The results show that the components in cyclohexanol residue include dicyclohexyl ether with a content of 84.33%and a boiling point of 242.5℃,3-cyclohexyl cyclohexene with a content of 4.80%and a boiling point of 230.4℃,1-cyclohexyl cyclohexene with a content of 5.29%and a boiling point of 234.2℃,and cyclohexylidenecyclohexane with a content of 5.58%and a boiling point of 237.6℃.The purity of dicyclohexyl ether extracted is up to 99.80%and total extraction rate is 93.9%.After extracting dicyclohexyl ether,the main components in the residue in the tower kettle include dicyclohexyl ether with a content of 86.30%and 1,1’-dihydroxydicyclohexyl with a content of 13.70%.

关 键 词：环己醇残液 二环己基醚 提取工艺 表征 

分 类 号：O656.22[理学—分析化学]