化工进展 ›› 2018, Vol. 37 ›› Issue (05): 1902-1907.DOI: 10.16085/j.issn.1000-6613.2017-1425

• 材料科学与技术 • 上一篇    下一篇

球磨法强化活性白土催化二聚酸合成

胡冬冬, 钱行, 计建炳, 陆向红   

  1. 浙江工业大学化工学院, 浙江 杭州 310014
  • 收稿日期:2017-07-10 修回日期:2017-08-16 出版日期:2018-05-05 发布日期:2018-05-05
  • 通讯作者: 陆向红,副教授,研究方向为生物质能源、过程强化、新型分离技术开发。
  • 作者简介:胡冬冬(1993-),男,硕士研究生。

Intensification of ball milling on the synthesis of dimer acid catalyzed by activated clay

HU Dongdong, QIAN Xing, JI Jianbing, LU Xianghong   

  1. College of Chemical Engineering, Zhejiang University of Technology, Hangzhou 310014, Zhejiang, China
  • Received:2017-07-10 Revised:2017-08-16 Online:2018-05-05 Published:2018-05-05

摘要: 采用球磨法强化白土催化制备二聚酸过程。以二聚酸的产率为评价指标,在球磨反应釜中考察了反应温度、催化剂用量、助催化剂用量、搅拌桨叶型式、搅拌速度、球磨介质用量对二聚酸合成的影响,并与搅拌釜的结果比较。结果表明:球磨法可以强化活性白土催化二聚酸合成过程,水蒸气氛围下,在反应温度260℃、催化剂质量分数24%、助催化剂质量分数0.5%,采用双螺旋带型桨叶、搅拌速度173r/min,球磨介质为氧化锆、球磨介质用量1500g(为原料质量的6倍)的反应条件下,制备得到二聚酸含量为79%、酸值为196mgKOH/g、黏度为1640mPa·s的二聚酸粗品,二聚酸产率为58.7%。相比于搅拌釜,球磨反应釜中二聚酸含量提高了75%。采用红外光谱(FTIR)、高效液相色谱-质谱(HPLC-Mass)等方法对产物进行表征,实验制得的二聚酸主要由双环二聚酸和无环二聚酸组成,双环二聚酸和无环二聚酸的比例为1.07∶1。

关键词: 聚合, 催化, 球磨, 制备, 二聚酸

Abstract: In this work,ball milling method was utilized to intensify the preparation process of dimer acid. The effects of reaction temperature,amount of catalyst,amount of co-catalyst,stirring blade type,stirring speed and amount of milling medium on the yield of dimer acid were investigated in the ball mill reactor. The results showed that the ball milling method can enhance the synthesis of dimer acid catalyzed by activated clay. A crude product with dimer acid content of 79%,acid value of 196mgKOH/g and viscosity of 1640mPa·s was prepared with water vapor when reaction temperature was 260℃,catalyst and cocatalyst amount was 24% and 0.5% respectively,a double propeller blade was used at the stirring speed of 173r/min,1500g zirconia was used as the milling medium,and the yield of dimer acid was 58.7%. Compared to the stirred tank,the content of dimer acid in the crude product was increased by 75% in the intensification of ball milling. The products were characterized by infrared spectroscopy (FTIR)and HPLC-Mass,the obtained dimer acid product is mainly composed of bicyclic dimer acid and acyclic dimer acid. The ratio of bicyclic dimer acid and acyclic dimer acid was 1.07:1.

Key words: polymerization, catalysis, ball milling, preparation, dimer acid

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