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林产化学与工业

林产化学与工业 ›› 2016, Vol. 36 ›› Issue (5): 68-74.doi: 10.3969/j.issn.0253-2417.2016.05.010

• 研究报告 • 上一篇    下一篇

阴离子型聚硅氧烷改性萜烯基环氧树脂多元醇水分散体的制备、表征及微观结构

刘迪1, 吴国民1,2, 刘贵锋1,2, 孔振武1,2   

  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. 中国林业科学研究院 林业新技术研究所, 北京 100091
  • 收稿日期:2015-12-23 出版日期:2016-10-25 发布日期:2016-11-05
  • 通讯作者: 孔振武,研究员,博士,博士生导师,主要从事生物质基聚合物材料的基础与应用技术研究;E-mail:kongzwlhs@163.com。 E-mail:kongzwlhs@163.com
  • 作者简介:刘迪(1989-),女,山东菏泽人,硕士生,主要从事天然资源化学与利用研究
  • 基金资助:
    国家林业局“948”项目（2015-04-43）

Preparation, Characterization and Micro-structure of Anionic Polysiloxane Modified Terpene-based Epoxy Resin Polyol Dispersion

LIU Di1, WU Guo-min1,2, LIU Gui-feng1,2, KONG Zhen-wu1,2   

  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. Research Institute of Forestry New Technology, CAF, Beijing 100091, China
  • Received:2015-12-23 Online:2016-10-25 Published:2016-11-05

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摘要： 以萜烯基环氧树脂（TME）与新戊二醇（NPG）反应，合成了萜烯基环氧树脂基多元醇（T-N），再以端羟丙基聚硅氧烷（HTP）、2，4-甲苯二异氰酸酯（TDI）及2，2-二（羟甲基）丙酸（DMPA）改性T-N，制备了阴离子型聚硅氧烷改性萜烯基环氧树脂多元醇（T-N-S）水分散体，并以红外光谱（FT-IR）、核磁共振光谱（NMR）表征了多元醇的化学结构。研究了反应条件、改性剂HTP用量等对多元醇水分散体稳定性及微观结构的影响。结果表明：DMPA与TDI物质的量比为1：2，丙酮为溶剂（用量为反应物总质量的1.5~2倍），丙酮回流温度（56℃）下反应3 h，再加入T-N及HTP，继续反应4 h，所合成的T-N-S能够较好地在水中分散。透射电子显微镜分析表明，当HTP用量为T-N质量的3%~12%时，制备的T-N-S水分散体粒子均为球形粒子，粒径范围100~300 nm。

关键词: 萜烯基环氧树脂, 端羟丙基聚硅氧烷, 多元醇水分散体, 微观结构

Abstract: Terpene-based epoxy resin polyol (T-N) was prepared via the reaction of terpene-based epoxy resin(TME) and neopentyl glycol(NPG). Then the T-N was modified with hydroxypropyl terminated polysiloxane(HTP), 2,4 tolylene diisocyanate(TDI) and 2,2-bis (hydroxymethyl) propionic acid(DMPA) to obtain the anionic polysiloxane-modified terpene-based epoxy resin polyol (T-N-S) dispersion. The chemical structure of the T-N-S was characterized by FT-IR and NMR. The micro-morphology of T-N-S was determined by transmission electron microscopy (TEM) and particles size measurement. And the effects of reaction condition and siloxane content on the stability and micro-structure of the polyol dispersion were studied. T-N-S dispersion was obtained at the conditions of DMPA and TDI were mixed with the molar ratio 1:2 in the presence of solvent acetone (the amount of solvent was 1.5-2 times based on the reactants mass) and refluxed at 56℃ for 3 h. Then HTP and T-N were added in to the reaction and continued to feflux for 4 h. The obtained T-N-S dispersion showed good stability and the particle size of the dispersion ranged from 100 to 300 nm when the dosage of HTP was 3%-12% of T-N by weight.

Key words: terpene-based epoxy resin, hydroxypropyl terminated polysiloxane, polyol dispersion, micro-structure

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