应用化学 ›› 2009, Vol. 26 ›› Issue (09): 1005-1010.

• 研究论文 •    下一篇

[AEIM]Cl的合成及微波溶解微晶纤维素

郭立颖,史铁钧,段衍鹏   

  1. (合肥工业大学化工学院 合肥 230009)
  • 收稿日期:2008-08-25 修回日期:2008-11-28 出版日期:2009-09-10 发布日期:2009-09-10
  • 通讯作者: 史铁钧,男,教授,博士生导师; E-mail:stjhfut@163.com; 研究方向:有机,无机杂化材料及高分子改性
  • 基金资助:
    国家自然科学基金(50773017)资助项目

Synthesis of [AEIM]Cl and its Solubility for Microcrystalline Cellulose by Microwave Heating Method

GUO Li-Ying, SHI Tie-Jun, DUAN Yan-Feng   

  1. (School of Chemical Engineering,Hefei University of Technology,Hefei 230009)
  • Received:2008-08-25 Revised:2008-11-28 Published:2009-09-10 Online:2009-09-10

摘要:

以氯丙烯和N-乙基咪唑为原料合成了离子液体氯化1-烯丙基-3-乙基-咪唑盐([AEIM]Cl),利用FT-IR和1HNMR对其化学结构进行了表征。采用微波加热法溶解微晶纤维素(MCC),考察 [AEIM]Cl对纤维素的溶解性能。研究了NaOH、微波和高压等3种预处理方式对微晶纤维素的相对结晶度、聚合度及溶解率的影响。利用FT-IR、XRD、TGA和SEM分别对溶解后得到的再生纤维素的化学结构、晶型变化、热稳定性及表观形貌进行测试与分析。结果表明,合成的离子液体是目标产物,对微晶纤维素表现出很好的溶解能力,且高温高压条件下15%的NaOH水溶液对微晶纤维素处理后,得到的纤维素相对结晶度最小,聚合度最低,溶解率最高。溶解过程中纤维素没有发生衍生化反应,溶解后得到的再生纤维素的相对结晶度和微晶尺寸变小,热稳定性降低。

关键词: 离子液体, 微晶纤维素, 溶解率, 结晶度, 聚合度, 再生纤维素

Abstract:

Abstract: Ionic liquid of 1-allyl-3-ethyl imidazolium chloride ([AEIM]Cl) had been synthesized using N-ethylimidazole and chloro-propene. The chemical structure of [AEIM]Cl was confirmed by FT-IR and 1HNMR. The solubility of [AEIM]Cl for microcrystalline cellulose (MCC) was studied by microwave heating method. Influences of pretreatment methods for MCC, such as NaOH, microwave and high pressure, on crystallinity, degree of polymerization (DP) and dissolution rate were studied. Chemical structure, change of crystal form, thermostability and appearance of the regenerated cellulose after dissolved were analyzed by FT-IR, XRD, TGA and SEM respectively. It showed that synthesis ionic liquid was the object product, which exhibited a very good soluble ability for MCC. Crystallinity of MCC was the smallest, DP was the lowest and dissolution rate was the highest on the condition of MCC pretreated with high pressure pot and 15% NaOH (mass fraction). Chemical reaction of MCC didn’t occur during the soluble process. The crystallinity of the regenerated cellulose decreased, and the thermostability declined.

Key words: ionic liquid, microcrystalline cellulose, dissolution rate, crystallinity, degree of polymerization, regenerated cellulose

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