洗油含芴馏分段反应-分离制9-芴酮工艺研究  

Study on Distillation Segmentation Containing Fluorene of Washing Oil to Produce 9-fluorenone Using Reaction-separation Method

作　　者：柴志方 桂欢欢 梁嘉欣 徐婕 韩信有 Chai Zhifang;Gui Huanhuan;Liang Jiaxin;Xu Jie;Han Xinyou(Shaanxi Coal Chemical Industry Technology Research Institute Co.,Ltd.,Xi′an 710100,China;State Energy Key Laboratory of Clean Coal Grading Conversion,Xi′an 710100,China)

机构地区：[1]陕西煤业化工技术研究院有限责任公司,陕西西安710100 [2]国家能源煤炭分质清洁转化重点实验室,陕西西安710100

出　　处：《山东化工》2024年第15期8-11,共4页Shandong Chemical Industry

基　　金：陕西煤业化工技术研究院自主研发项目(2022YJY-Y-ZZ-XS-HG002)。

摘　　要：为了提高洗油中芴的利用率,分别以模拟和真实含芴馏分段为原料,采用反应-分离的新工艺进行了直接氧化制9-芴酮的工艺研究。结果表明:在最佳工艺条件下(原料与溶剂质量比1∶7,进气速率250 mL/min,催化剂用量5%,反应温度40℃),15 min内即可实现模拟原料中芴的完全转化;而对于真实原料,在相同工况下,反应速率明显变慢,通过增加催化剂用量可明显缩短反应时间。反应后9-芴酮混合物通过精馏即可得到纯度>95%的9-芴酮粗品,再结合重结晶工艺可得到纯度>99%的9-芴酮产品。与传统分离-反应工艺相比,本工艺9-芴酮产品总收率可提高近6%。In order to improve the utilization of fluorene in washing oil,a new reaction-separation method was used to directly prepare 9-fluorenone using model and real distillation segmentation containing fluorene as raw materials respectively.The results showed that,under the optimal conditions(raw material to solvent mass ratio of 1∶7,gas rate of 250 mL/min,catalyst dosage of 5%,reaction temperature of 40℃),for model materials,the fluorene could be completely converted to 9-fluorenone within 15 min.However,for real materials,the reaction rate decreased significantly under the same conditions.The reaction time could be shortened by increasing catalyst dosage.The crude product of 9-fluorenone with a purity greater than 95%could be obtained from the mixture after reaction by distillation method.Combined with recrystallization process,the 9-fluorenone product with a purity greater than 99%could be obtained.Compared with the traditional separation-reaction method,the total yield of 9-fluorenone using this method can increase by nearly 6%.

关 键 词：洗油 含芴馏分段 9-芴酮 反应-分离 

分 类 号：TQ522.6[化学工程—煤化学工程]