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日用化学工业（中英文）

日用化学工业 ›› 2022, Vol. 52 ›› Issue (6): 594-600.doi: 10.3969/j.issn.1001-1803.2022.06.003

• 开发与应用 • 上一篇    下一篇

脱氢枞氧基聚氧乙烯缩水甘油醚接枝羟乙基壳聚糖制备及其表面活性

黄旭娟1,王婷1,丁正青1,杨欣欣2,蔡照胜1,*(),商士斌2   

  1. 1.盐城工学院 化学化工学院,江苏 盐城 224000
    2.中国林业科学研究院 林产化学工业研究所,江苏 南京 210042
  • 收稿日期:2021-09-28 修回日期:2022-05-30 出版日期:2022-06-22 发布日期:2022-06-22
  • 通讯作者: 蔡照胜
  • 基金资助:
    国家自然科学基金面上基金资助项目(32071706);国家自然科学基金青年基金项目(31901257)

Preparation and surface-active properties of dehydroabietyl polyoxyethylene glycidyl ether grafted hydroxyethyl chitosan

Huang Xujuan1,Wang Ting1,Ding Zhengqing1,Yang Xinxin2,Cai Zhaosheng1,*(),Shang Shibin2   

  1. 1. School of Chemistry and Chemical Engineering, Yancheng Institute of Technology, Yancheng, Jiangsu 224000, China
    2. Institute of Chemical Industry of Forest Products, Chinese Academy of Forestry, Nanjing, Jiangsu 210042, China
  • Received:2021-09-28 Revised:2022-05-30 Online:2022-06-22 Published:2022-06-22
  • Contact: Zhaosheng Cai

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摘要：

脱氢枞醇聚氧乙烯（5）醚（DA（EO） 5H）在BF3·乙醚催化下与环氧氯丙烷缩合后,再在NaOH存在下使生成的缩合产物进行分子内脱氯化氢,得到脱氢枞氧基聚氧乙烯（5）缩水甘油醚（DA（EO） 5GE）;然后通过DA（EO） 5GE与水溶性羟乙基壳聚糖（HECTS）间的亲核加成反应,得到以氢化菲环为主要亲油基、HECTS为主要亲水基和聚氧乙烯链为辅助亲水亲油结构的高分子表面活性剂DA（EO） 5GE接枝HECTS（DA（EO） 5GE-g-HECTS）。用FT-IR、1H NMR和UV-Vis表征了接枝产物结构,元素分析法测定了其接枝度（DG）,表面张力法和乳液稳定时间法分别研究了产物的表面活性和乳化能力。结果表明：利用不同原料比,可以制备得到具有不同接枝度的DA（EO） 5GE-g-HECTS。当DA（EO） 5GE-g-HECTS的DG从12.98 %增加至31.73%时,其临界胶束浓度（cmc）从0.378 g/L降至0.249 g/L,对液体石蜡-水乳液的乳化能力呈现先增强后减弱的趋势;以1.0 g/L的DA（EO） 5GE-g-HECTS4（DG为28.33%）水溶液与等体积液体石蜡形成的乳液,其稳定时间为565 s,优于TX-10为稳定剂时的165 s。

关键词: 脱氢枞氧基聚氧乙烯缩水甘油醚, 羟乙基壳聚糖, 接枝改性, 表面活性

Abstract:

Dehydroabietol polyoxyethylene（5） ether （DA（EO）5H） was condensated with epichlorohydrin in the presence of boron fluoride diethyl etherate firstly. Then, dehydroabietyl polyoxyethylene glycidyl ether （DA（EO） 5GE） was obtained through dehydrochlorination of the condensation product in the presence of NaOH. Finally, DA（EO） 5GE grafted hydroxyethyl chitosan （DA（EO） 5GE-g-HECTS）, a polymeric surfactant with hydrogenate phenanthrene ring as main lipophilic group, sugar chain of hydroxyethyl chitosan （HECTS） as main hydrophilic group, and polyoxyethylene chain as assist lipophilic-hydrophilic structure, was prepared through the grafting modification of DA（EO） 5GE to water-soluble HECTS. The structure of the grafted product was characterized by Fourier transform infrared （FT-IR）, 1H nuclear magnetic resonance 1H NMR and UV-Vis spectrophotometry. The grafting degree （DG） of products were characterized using elemental analysis, and their surface-active activities and emulsifying capacity were investigated using surface tension method and emulsion stabilization time method, respectively. The result show that the DA （EO） 5GE-g-HECTS with different DG can be prepared by using different raw material ratio. When the DG of DA（EO） 5GE-g-HECTS increases from 12.98% to 31.73%, the critical micelle concentration （cmc） decreases from 0.378 g/L to 0.249 g/L. The emulsions are prepared by blending 50% （φ/%） liquid paraffin and 50% （φ/%） DA（EO） 5GE-g-HECTS aqueous suspensions. The emulsifying capacity of DA（EO） 5GE-g-HECTS increases at first and then decreases with the increasing DG. When the DA（EO）5GE-g-HECTS4 （its DG is 28.33% and the mass concentration is 1.0 g/L） is utilized as emulsifier, the stability time of emulsion composed of liquid paraffin and water is 565 s. It is better than the TX-10 emulsifier which is 165 s at the same condition.

Key words: dehydroabietyl polyoxyethylene glycidyl ether, hydroxyethyl chitosan, grafting modification, surface-active activity

中图分类号: 

  • TQ281