华南理工大学学报(自然科学版) ›› 2025, Vol. 53 ›› Issue (11): 1-.doi: 10.12141/j.issn.1000-565X.240368

• 化学化工 •    

煤制乙二醇悬浮结晶精制试验研究

薛雨源  赵淼  赵志仝  袁栋勇  李钢   

  1. 太原理工大学 化学与化工学院,山西 太原  030024

  • 出版日期:2025-11-25 发布日期:2025-01-17

Experimental Study on Suspension Crystallization Refining of Coal-to-Ethylene Glycol

XUE Yuyuan  ZHAO Miao  ZHAO Zhitong  YUAN Dongyong  LI Gang   

  1. Taiyuan University of Technology, College of Chemistry and Chemical Engineering, Shanxi Taiyuan, 030024
  • Online:2025-11-25 Published:2025-01-17

摘要:

悬浮结晶耦合离心分离可精制获得聚酯级煤制乙二醇。基于煤制乙二醇生产工艺中杂质与乙二醇形成窄沸、共沸以及热敏体系,与传统精馏纯化相比,悬浮结晶的低能耗、无需溶剂、对环境友好等优点,在纯化该体系下能达到节能减排的效果。操作工艺优化可为悬浮结晶耦合离心分离技术开发提供参考。本文研究了晶种添量、滤饼厚度、搅拌强度、程序降温和母液循环操作工艺对纯化效果的影响。结果显示,晶种添量对晶体的粒径分布产生影响,晶种添量增大可提升产品纯度,有效分配系数降幅为15.8%;降低滤饼厚度,晶体与发汗气体接触更充分,发汗效果增强,有效分配系数最大降幅为56.8%;搅拌强度直接影响传质传热,搅拌强度越大,产品纯度越高,但收率随之下降,有效分配系数和收率最大降幅分别为39.4%和30.8%;程序降温直接影响结晶时间,结晶时间增加,程序降温反而降低产品纯度;母液循环使用导致体系水含量增加,降低过冷度,反而提升了产品纯度,与新鲜母液相比,循环7次时有效分配系数降低了72.0%。

关键词: 煤制乙二醇, 聚酯级, 悬浮结晶, 工艺优化

Abstract:

Suspension crystallization coupled centrifugal separation can directly prepare polyester grade coal-to-ethylene glycol. Based on the narrow boiling, azeotropic and heat sensitive system formed by impurities and ethylene glycol in the production process of coal to ethylene glycol, compared with the traditional distillation purification, suspension crystallization has the advantages of low energy consumption, no solvent and environmental friendly, and can achieve the effect of energy saving and emission reduction under the purification system. The optimization of crystallization operation can provide a reference for suspension crystallization coupled centrifugal separation technology. The effects of seed addition, filter cake thickness, stirring intensity, programmed cooling and mother liquor circulation operation process on the purification effect were studied. The results show that the particle size distribution of crystals is affected by the amount of seed addition. The purity of the product can be improved by increasing the amount of seed added, and the distribution coefficient can be reduced by about 15.8%; Because crystal and sweat gas more fully contact, reduced cake thickness enhances sweating with a maximum reduction of 56.8% distribution coefficient; Stirring intensity directly affects mass and heat transfer. The higher the stirring intensity, the higher the purity of the product, but the yield decreased, and the maximum decrease in distribution coefficient and yield was 39.4% and 30.8%, respectively; Programmed cooling directly affects crystallization time. Due to the increase of crystallization time, the program cooling reduces the purity of the product; The recycling of mother liquor led to the increase of water content in the system, which reduced the degree of under cooling, but improved the purity of the product, and the distribution coefficient decreased by 72.0% when it was cycled for 7 times compared with the fresh mother liquor.

Key words: coal-to-ethylene glycol, polyester grade, suspension crystallization, process optimization