山东化工2024,Vol.53Issue(15) :8-11.

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

柴志方 桂欢欢 梁嘉欣 徐婕 韩信有
山东化工2024,Vol.53Issue(15) :8-11.

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

柴志方 1桂欢欢 1梁嘉欣 1徐婕 1韩信有1
扫码查看

作者信息

  • 1. 陕西煤业化工技术研究院有限责任公司,陕西西安 710100;国家能源煤炭分质清洁转化重点实验室,陕西西安 710100
  • 折叠

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℃),15min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%.

Abstract

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 mir..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

Key words

washing oil/distillation segmentation containing fluorene/9-fluorenone/reaction-separation

引用本文复制引用

出版年

2024
山东化工
山东省化工研究院 山东省化工信息中心

山东化工

影响因子:0.249
ISSN:1008-021X
段落导航相关论文