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日用化学工业（中英文） ›› 2026, Vol. 56 ›› Issue (3): 323-332.doi: 10.3969/j.issn.2097-2806.2026.03.006

• 基础研究 • 上一篇    下一篇

四甲氧甲基甘脲合成工艺及宏观动力学的研究

王为尚1,2,崔文华2,*(),王潇潇1,薛永兵1,刘振民1   

  1. 1 太原科技大学 化学工程与技术学院， 山西 太原 030024
    2 太原科源达精细化工有限公司， 山西 太原 030400
  • 收稿日期:2025-04-28 修回日期:2026-03-03 出版日期:2026-03-22 发布日期:2026-05-14
  • 通讯作者: 崔文华
  • 基金资助:
    山西省基础研究计划(202103021223294);山西省重点研发计划项目(201903D121025);山西省研究生教育创新项目(2022Y707)

Study on the synthesis process and macro-kinetics of tetramethoxymethylglycoluril

Weishang Wang1,2,Wenhua Cui2,*(),Xiaoxiao Wang1,Yongbing Xue1,Zhenmin Liu1   

  1. 1 College of Chemical Engineering and Technology, Taiyuan University of Science and Technology, Taiyuan, Shanxi 030024, China
    2 Taiyuan Keyuanda Fine Chemical Co., Ltd., Taiyuan, Shanxi 030400, China
  • Received:2025-04-28 Revised:2026-03-03 Online:2026-03-22 Published:2026-05-14
  • Contact: Wenhua Cui

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摘要：

研究在500 mL间歇反应釜内甘脲及四甲氧甲基甘脲（TMMG）的合成反应。采用正交试验设计法优化合成工艺，结果表明，甘脲较优合成条件为：尿素与乙二醛摩尔比2.5∶1、pH=1.2、反应温度60 ℃、保温时间3 h，产率为91.79%，经液相色谱检测其纯度达到99%；TMMG较优合成工艺为：THMG与甲醇摩尔比1∶12、反应温度50 ℃、反应时间2 h，产率为86.54%，经液相色谱检测其纯度达到99.92%。通过宏观动力学分析，甘脲合成反应中尿素的反应级数为0.425，乙二醛的反应级数为1.637，该反应的总级数为2.06，活化能为87.446 kJ/mol。TMMG合成时一般甲醇过量，该反应表现为准一级反应，反应的活化能为87.345 kJ/mol。产物结构及纯度经¹H NMR、FT-IR、熔点仪及HPLC验证符合工业标准。本研究为产物在日化用品及光刻胶领域的应用提供理论依据。

关键词: 甘脲, 四甲氧甲基甘脲, 动力学, 阿伦尼乌斯方程

Abstract:

The syntheses of glycoluril and tetramethoxymethylglycoluril （TMMG） in a 500 mL batch reactor were investigated. Orthogonal experimental design method was used for process optimization. The results showed that the optimized conditions for synthesis of glycoluril were as follows: Under the conditions of the molar ratio of urea-to-glyoxal of 2.5∶1, pH of 1.2, reaction temperature of 60 ℃, and holding time of 3 h, the yield was 91.79% and the purity of product was 99% as confirmed by HPLC. For synthesis of TMMG, the optimized parameters were as follows: The molar ratio of methanol-to-precursor was 12∶1, the reaction temperature was 50 ℃, and the reaction time was 2 h, producing a yield of 86.54% and the purity of 99.92% as confirmed by HPLC. Macrokinetic analysis demonstrated that the reaction orders were 0.425 for urea and 1.637 for glyoxal in synthesis of glycoluril, indicative of an overall reaction order of 2.06 and activation energy of 87.446 kJ/mol. The synthesis of TMMG followed pseudo-first-order kinetics under methanol-excess conditions with an activation energy of 87.345 kJ/mol. The products were characterized by using 1H NMR, FT-IR, melting point analysis and HPLC, which confirmed that the products met industrial specifications. This study could provide theoretical support for applications in daily chemicals and photoresist materials.

Key words: glycoluril, tetramethoxymethylglycoluril, kinetics, Arrhenius formula

中图分类号: 

  • TQ437