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生物质化学工程 ›› 2019, Vol. 53 ›› Issue (1): 1-7.doi: 10.3969/j.issn.1673-5854.2019.01.001

• 研究报告 •    下一篇

N-甲基-N, N-二烯丙基-N-(3-脱氢枞酰氧基)丙基溴化铵的合成及其自聚动力学分析

张海波1,2(),蒋建新2,商士斌1,*(),宋湛谦1   

  1. 1. 中国林业科学研究院 林产化学工业研究所;生物质化学利用国家工程实验室;国家林业局 林产化学工程重点开放性实验室;江苏省 生物质能源与材料重点实验室,江苏 南京 210042
    2. 北京林业大学 材料科学与技术学院,北京 100083
  • 收稿日期:2017-11-21 出版日期:2019-01-30 发布日期:2019-03-15
  • 通讯作者: 商士斌 E-mail:shdzhanghaibo@163.com;shangsb@hotmail.com
  • 作者简介:张海波(1989—),男,山东菏泽人,博士,研究方向:生物质化学与利用; E-mail:shdzhanghaibo@163.com
  • 基金资助:
    国家自然科学基金资助项目(31470597);中国林科院林产化学工业研究所研究团队建设创新工程项目(LHSXKQ1)

Preparation and Self-polymerization Kinetics of N-methyl-N, N-divinyl-3-dehydroabietoyloxypropan-1-ammonium Bromide

Haibo ZHANG1,2(),Jianxin JIANG2,Shibin SHANG1,*(),Zhanqian SONG1   

  1. 1. Institute of Chemical Industry of Forest Products, CAF; National Engineering Lab. for Biomass Chemical Utilization; Key and Open Lab. of Forest Chemical Engineering, SFA; Key Lab. of Biomass Energy and Material, Jiangsu Province, Nanjing 210042, China
    2. College of Materails Science and Technology, Beijing Forestry University, Beijing 100083, China
  • Received:2017-11-21 Online:2019-01-30 Published:2019-03-15
  • Contact: Shibin SHANG E-mail:shdzhanghaibo@163.com;shangsb@hotmail.com
  • Supported by:
    国家自然科学基金资助项目(31470597);中国林科院林产化学工业研究所研究团队建设创新工程项目(LHSXKQ1)

摘要:

以脱氢枞酸、3-溴-1-丙醇、甲基二烯丙基胺为原料制备了水溶性松香单体N-甲基-N, N-二烯丙基-N-(3-脱氢枞酰氧基)丙基溴化铵(DMDHAE),并使用核磁共振、气相色谱、元素分析、红外光谱、质谱、熔点仪等分析手段对合成产物的结构和性质进行了定量和定性分析。结果表明:所合成的DMDHAE纯度为91%,熔点为127~131℃,溶解度为1.50~1.60 g/mL;核磁和红外分析中出现了特征基团峰,质谱和元素分析与理论值一致。采用差示扫描量热仪对单体自聚进行监测,并利用自催化模型对其自聚动力学进行了研究。结果表明:DMDHAE具有可聚性,单体自聚的活化能(Ea)为124.336 kJ/mol,机理函数f(α)的表达式为SB(m, n)模型。

关键词: N-甲基-N, N-二烯丙基-N-(3-脱氢枞酰氧基)丙基溴化铵, 松香, 合成, 聚合动力学

Abstract:

Water-soluble rosin monomer N-methyl-N, N-divinyl-3-dehydroabietoyloxypropan-1-ammonium bromide(DMDHAE) was prepared from dehydroabietic acid, 3-bromopropanol and methyldiallylamine, and its structure was characterized by nuclear magnetic resonance(NMR), gas chromatography(GC), elemental analysis, FT-IR, mass spectrometry(MS) and melting point instrument. The results indicated that the purity of monomer was 91%, melting point was 127-131 ℃, and solubility was 1.50-1.60 g/mL; characteristic group peaks were appeared in the NMR and FT-IR spectra, and the mass spectrometry and elemental analysis results were consistent with the theoretical value. The self-polymerization parameter was measured by differential scanning calorimeter(DSC), and self-polymerization kinetics was analyzed with autocatalytic model. The results showed that DMDHAE was polymerizability, the activation energy(Ea) was 124.336 kJ/mol, and mechanism function f(α) was SB(m, n) model.

Key words: N-methyl-N, N-divinyl-3-dehydroabietoyloxypropan-1-ammonium bromide, rosin, synthesis, polymerization kinetics

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