刘志雷,周街胜,周建萍,刘光明.纳米 SiO2 表面“点击”化学法接枝共聚物[J].表面技术,2015,44(7):34-39.
LIU Zhi-lei,ZHOU Jie-sheng,ZHOU Jian-ping,LIU Guang-ming.Copolymer Modified Nano-silica via ‘Click' Chemistry[J].Surface Technology,2015,44(7):34-39
纳米 SiO2 表面“点击”化学法接枝共聚物
Copolymer Modified Nano-silica via ‘Click' Chemistry
投稿时间:2015-03-10  修订日期:2015-07-20
DOI:10.16490/j.cnki.issn.1001-3660.2015.07.007
中文关键词:  纳米 SiO2  “点击”化学法  分散性  接枝  共聚物
英文关键词:nanometer silica  ‘click' chemistry  dispersion  graft  copolymer
基金项目:国家自然科学基金(51303078,51363017)
作者单位
刘志雷 南昌航空大学 材料科学与工程学院, 南昌 330000 
周街胜 南昌航空大学 材料科学与工程学院, 南昌 330000 
周建萍 南昌航空大学 材料科学与工程学院, 南昌 330000 
刘光明 南昌航空大学 材料科学与工程学院, 南昌 330000 
AuthorInstitution
LIU Zhi-lei School of Materials Science and Engineering, Nanchang Hangkong University, Nanchang 330000, China 
ZHOU Jie-sheng School of Materials Science and Engineering, Nanchang Hangkong University, Nanchang 330000, China 
ZHOU Jian-ping School of Materials Science and Engineering, Nanchang Hangkong University, Nanchang 330000, China 
LIU Guang-ming School of Materials Science and Engineering, Nanchang Hangkong University, Nanchang 330000, China 
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中文摘要:
      目的 提高纳米 SiO2 在有机溶剂及树脂基体中的分散性。 方法 首先利用普通自由基聚合的方式制备苯乙烯及马来酸酐共聚物(PSMA),再与丙炔醇反应,在分子链上引入多个炔基,然后利用硅烷偶联剂 KH560 改性纳米 SiO2,之后与叠氮化钠反应,在纳米 SiO2 粒子表面引入多个叠氮基团,最后将带有多个炔基的分子链通过“点击”化学接枝到纳米 SiO2 表面。 结果 酸碱反滴定法测得聚合物中马来酸酐的质量分数为 26. 5% 。 凝胶渗透色谱测得聚合物数均相对分子质量为 36200,相对分子质量分布为1. 39。 红外表征显示,聚合物上带有多个炔基,纳米 SiO2 粒子表面带有多个叠氮基,经过 24 h“点击”化学反应,聚合物成功接枝到粒子表面,同时叠氮基吸收峰消失。 热重(TG)结果表明,接枝率为 32. 83% 。扫描电镜分析表明,接枝聚合物后,粒子的分散性增强。 结论 分子链上含有多个炔基的共聚物(PSMA)通过“点击”化学反应成功接枝到了纳米 SiO2 粒子表面,不会引起粒子间的交联,可以明显提高纳米 SiO2粒子在有机溶剂中的分散性。
英文摘要:
      Objective To improve the dispersion of nano-silica in organic solvents and resin matrix. Methods Firstly, styrenemaleic anhydride copolymer (PSMA) was synthesized by common free radical polymerization. Then, the copolymer was reacted with propargyl alcohol to introduce multiple alkynyl groups. Nano-silica was firstly modified by silane coupling agent (KH560), then reacted with sodium azide to introduce azide groups. Finally, the copolymer (PSMA) with multiple alkynyl was grafted onto the surface of nano-silica via ‘click' chemistry. Results The mass fraction of maleic anhydride in polymer was 26. 5% measured by neutralization titration. The number average molecular weight of the polymer was 36200 and the molecular weight distribution was 1. 39 analyzed by gel permeation chromatography. Analysis by IR ( FT-IR) indicated that there were multiple alkynyl on the copolymer, and multiple azide on the surface of nano-silica. After ‘click' chemical reaction for 24 hours, the copolymer was grafted onto nano-silica with disappearance of characteristic absorption peaks of azide groups. Analysis of SEM and TG conformed that 32. 83% copolymer (PSMA) was grafted onto nano-silica, and scanning electron microscopy showed the dispersion was improved after the graft. Conclusion Copolymer (PSMA) with multiple active alkynyl groups can be grafted onto nano-silica via ‘click' chemistry successfully with no occurrence of particle cross-linking, and the dispersion of nano-silica in organic solvents was improved obviously.
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