Chemical Industry and Engineering Progress ›› 2018, Vol. 37 ›› Issue (S1): 187-192.DOI: 10.16085/j.issn.1000-6613.2018-0694

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Preparation of diethylene glycol vinyl ether by liquid phase cyclic reaction in tubular reactor

HUANG Xinquan, LI Sifang   

  1. College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005, Fujian, China
  • Received:2018-04-03 Revised:2018-05-28 Online:2018-12-13 Published:2018-11-30

管式反应器液相循环反应制备二甘醇乙烯基醚

黄心权, 黎四芳   

  1. 厦门大学化学化工学院, 福建 厦门 361005
  • 通讯作者: 黎四芳,教授,研究方向为精细化工。
  • 作者简介:黄心权(1992-),男,硕士研究生。

Abstract: Using potassium diethylene glycolate as catalyst, diethylene glycol vinyl ether was synthesized from acetylene and diethylene glycol by liquid phase cyclic reaction in a tubular reactor. The effects of catalyst dosage, reaction temperature, reaction pressure and residence time on acetylene conversion were studied. The appropriate reaction conditions are as following:the dosage of potassium diethylene glycolate is 4% based on diethylene glycol mass, the reaction temperature is 175℃, the reaction pressure is 6MPa and the residence time is 175s. Under these conditions, continuous production of diethylene glycol were conducted. At steady state, the conversion of diethylene glycol reached 76.03%, the yield of diethylene glycol monovinyl ether was 59.03%, the yield of diethylene glycol divinyl ether was 15.10% and the total yield of diethylene glycol vinyl ether was up to 74.13%. The reaction of diethylene glycol and acetylene was in good agreement with the first order reaction kinetics. The pre-exponential factor k0 is 1.20×108s-1, and the reaction activation energy E is 86.86kJ/mol. Because of no existence of gas-phase acetylene in the tubular reactor, the danger of flammable and explosive acetylene in the gas phase under high temperature and high pressure has been overcome.

Key words: reactors, diethylene glycol vinyl ether, acetylene, reaction kinetics, preparation

摘要: 以乙炔和二甘醇为原料,二甘醇钾为催化剂,采用管式反应器液相循环反应制备二甘醇乙烯基醚。研究了催化剂用量、反应温度、反应压力和停留时间等因素对乙炔转化率的影响,得到较为适宜的反应条件为:催化剂二甘醇钾用量为二甘醇质量的4%、反应温度175℃、反应压力6MPa、停留时间175s。在该条件下进行了液相连续循环反应,反应达到稳态时,二甘醇的转化率为76.03%,二甘醇单乙烯基醚收率为59.03%,二甘醇双乙烯基醚的收率为15.10%,合计二甘醇乙烯基醚总收率为74.13%。单位反应体积二甘醇乙烯基醚的产率为143.2g/(h·mL)。二甘醇与乙炔反应符合一级反应动力学方程,反应的指前因子k0=1.20×108s–1,反应的活化能E=86.86kJ/mol。管式反应器中无气相乙炔,克服了高温高压下气相乙炔易燃易爆的危险。

关键词: 反应器, 二甘醇乙烯基醚, 乙炔, 反应动力学, 制备

CLC Number: 

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