PMDA-6FHP-DR1/SiO2杂化纳米材料的结构设计和合成

doi:10.7517/j.issn.1674-0475.2005.02.136

影像科学与光化学 ›› 2005, Vol. 23 ›› Issue (2): 136-143.DOI: 10.7517/j.issn.1674-0475.2005.02.136

PMDA-6FHP-DR1/SiO₂杂化纳米材料的结构设计和合成

邱凤仙^1,2, 周钰明¹, 刘举正¹, 张旭苹³

1. 东南大学, 化学化工系, 江苏, 南京210096;
2. 江苏大学, 化学化工学院, 江苏, 镇江, 212013
3. 南京大学, 光通信工程研究中心, 江苏, 南京210093

收稿日期:2004-09-10 修回日期:2004-12-27 出版日期:2005-03-23 发布日期:2005-03-23
通讯作者: 邱凤仙
基金资助:
国家自然科学基金资助项目(50377005,60277020);江苏省自然科学基金(BK2003064);江苏大学微纳米科学技术研究开放基金(1291400001).

Structural Design and Synthesis of PMDA-6FHP-DR1/SiO₂ Hybrid Nanomaterial

QIU Feng-xian^1,2, ZHOU Yu-ming¹, LIU Ju-zheng¹, ZHANG Xu-ping³

1.Department of Chemistry and Chemical Engineering, Southeast University, Nanjing 210096, Jiangsu, P.R.China;
2. School of Chemistry and Chemical Engineering, Jiangsu University, Zhenjiang 212013, Jiangsu, P.R.China;
3. Institute of Optical Communication Engineering, Nanjing University, Nanjing 210093, Jiangsu, P.R.China

Received:2004-09-10 Revised:2004-12-27 Online:2005-03-23 Published:2005-03-23

摘要/Abstract

摘要： 以含氟的二胺5,5'-(六氟异丙基)-二-(2 氨基苯酚)及均苯四甲酸酐 (PMDA)为单体,首先合成了经酰胺化的主链上带有活性羟基的含氟聚酰亚胺,再通过Mitsunobu反应将活性生色分子分散红1 (DR1)共价链接到聚酰亚胺的侧链骨架上,合成了含氟聚酰亚胺.采用溶胶凝胶 (Sol-Gel)技术,并利用偶联剂γ-氨丙基三乙氧基硅烷 (APTES)制备带有发色团的和含有硅氧烷端分子的聚酰胺酸,其中的Si (OR)₃基经水解、缩合后,与正硅酸乙酯 (TEOS)在催化剂作用下反应,经杂化、凝胶后,得到光学透明且热稳定性高的有机/无机杂化材料.将制得的含氟聚酰亚胺/SiO₂杂化材料,采用红外光谱 (FT-IR)、扫描电子显微镜 (SEM)、透射电子显微镜 (TEM)、X射线衍射 (XRD)、示差扫描量热法 (DSC),对材料的结构、表面形貌、热性能进行了表征.

关键词: 聚酰亚胺, 杂化材料, 均苯四甲酸酐, 偶联剂

Abstract: The fluorine-containing monomers 2,2-bis (3-amino-4-hydroxy phenyl) hexafluoropropane (6FHP) and pyromellitic dianhydride (PMDA) were used. It is a first-step preparation of a preimided hydroxy-containing polyimide, followed by the covalent bonding of an active chromophore dispered red 1 (DR1) onto the backbone of the polyimide via the Mitsunobu reaction. The fluorine-containing polyimide was synthesized. Then, Sol-Gel technique was adopted, utilizing 3-aminopropyltriethoxysilane (APTES) as a coupling agent, poly (amide acid), containing chromophore and alkoxysilane monomers, was synthesized. Si (OR)₃ group was hydrolyzed and condensated. It reacted with Tetraethoxysilane (TEOS) in presence of catalyst, via hybridization and gelation. The hybrid material was obtained with optics transparent, nonlinear optical, high thermal stability. Fluorine-containing polyimides/silica hybrid material was characterized by the methods of FT-IR spectra, Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM), X-Ray Diffraction (XRD), Differential Scanning Calorimetry (DSC) measuring apparatus to get their surface structure, morphology, thermal performance.

Key words: polyimide, Sol-Gel process, pyromellitic dianhydride (PMDA), coupling agent

中图分类号:

O631

邱凤仙, 周钰明, 刘举正, 张旭苹. PMDA-6FHP-DR1/SiO₂杂化纳米材料的结构设计和合成[J]. 影像科学与光化学, 2005, 23(2): 136-143.

QIU Feng-xian, ZHOU Yu-ming, LIU Ju-zheng, ZHANG Xu-ping. Structural Design and Synthesis of PMDA-6FHP-DR1/SiO₂ Hybrid Nanomaterial[J]. Imaging Science and Photochemistry, 2005, 23(2): 136-143.

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PMDA-6FHP-DR1/SiO₂杂化纳米材料的结构设计和合成

Structural Design and Synthesis of PMDA-6FHP-DR1/SiO₂ Hybrid Nanomaterial

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