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Continuous Flow Preparation of 2,2,4-trimethyl-1,3-pentanediol and its Kinetics
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Jilin Institute of Chemical Technology, Jilin 132000, China

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    Abstract:

    In order to improve the economic benefit of producing 2,2,4-trimethyl-1,3-pentanediol(TMDP), a more efficient and safe microchannel continuous flow process was selected to replace the traditional kettle-type batch production method with using isobutyl aldehyde as raw material and sodium hydroxide solution as catalyst. The effects of catalyst sodium hydroxide concentration, dosage, temperature and residence time on the reaction were investigated. The optimum conditions were determined as follows: sodium hydroxide concentration 50%, v(isobutyral)∶v(NaOH)=1, residence time 10 min, reaction temperature 40 ℃. Under these conditions, the conversion of isobutyraldehyde was 99.02%, the selectivity of TMDP was 93.57%, and the yield was 92.65%. The process made full use of the excellent mass and heat transfer characteristics of the microchannel reactor, greatly shortened the reaction time, increased the reaction rate, extended the selection range of process conditions, and realized the effective control of the reaction process of hydroxylaldehyde condensation. At the same time, the kinetic studies were carried out at different temperatures and concentrations of sodium hydroxide, and the kinetic equations and corresponding parameters were obtained with the concentration of sodium hydroxide being 50% and 45% respectively. The macroscopic kinetics obtained by fitting is second-order, and the activation energy and pre-exponential factors are: 26.34 kJ·mol-1, 2888.26 L·K-1·mol-1·min-1.

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李瑞端,潘宵,栗晓宁,等.微通道反应器中合成2,2,4-三甲基-1,3-戊二醇的连续流工艺及其动力学[J].含能材料,2022,30(5):424-430.
LI Rui-duan, PAN Xiao, LI Xiao-ning, et al. Continuous Flow Preparation of 2,2,4-trimethyl-1,3-pentanediol and its Kinetics[J]. Chinese Journal of Energetic Materials,2022,30(5):424-430.

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History
  • Received:January 21,2022
  • Revised:April 20,2022
  • Adopted:April 07,2022
  • Online: April 11,2022
  • Published: May 25,2022