PMDA-6FHP-DR1/SiO_2杂化纳米材料的结构设计和合成

Structural Design and Synthesis of PMDA-6FHP-DR1/SiO_2 Hybrid Nanomaterial

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.

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.