发布时间 : 星期一 文章聚酰亚胺、SIO2复合膜材料的制备与研究(1)更新完毕开始阅读88e749ffcd22bcd126fff705cc17552707225e2c
辽宁科技大学本科生论文 第I页 聚酰亚胺/二氧化硅纳米复合材料膜的研究
摘 要
本实验采用二酐单体1,2,3,4-环丁烷四羧酸二酐（CBDA）与二胺单体1,4-双(2-三氟甲基-4-氨基苯氧基)苯（6FAPB）为原料以N,N-二甲基乙酰胺（DMAc）为溶剂制备纯的聚酰胺酸（PAA）溶液。通过涂膜固化、程序化升温进行酰亚胺化，得到纯的聚酰亚胺(PI)薄膜，并确定酰亚胺化工艺。然后，在制备纯的PAA的基础上，添加正硅酸四乙酯（TEOS），进行溶胶-凝胶（Sol-gel）反应，通过热酰亚胺化工艺，制备出不同二氧化硅(SiO2)含量的聚酰亚胺/二氧化硅（PI/SiO2）复合材料薄膜。在不同二氧化硅(SiO2)含量加水浓酸催化和加水不加酸催化的条件下，自成三个体系PI/SiO2/H2O、PI/SiO2/H2O/H2SO4和PI/SiO2，与纯的聚酰亚胺(PI)薄膜分别比较水解对薄膜特性的影响。最后，利用紫外-可见光谱(UV-Vis)、红外光谱(IR)、热失重分析(TGA)测试方法研究了此类材料的结构与性能。实验结果表明：随着SiO2含量的增加，PI/SiO2薄膜的透明性逐渐降低，加水不加酸体系的透明性高于加水加酸体系。
关键词：聚酰亚胺；二氧化硅；溶胶-凝胶；纳米复合材料
辽宁科技大学本科生论文 第II页
Abstract
In this experiment, the alicyclic dianhydride 1,2,3,4-cyclobutane dianhydride (CBDA) and the monomer diamine 1,4-bis (2 – trifluoromethyl-4-aminophenoxy ) benzene (6FAPB) as raw material for N, N-dimethylacetamide (DMAc) as solvent and preparation of pure poly(amic acid)(PAA) solution. Cured through the film, and procedures of imidization process temperature to get pure polyimide (PI) film. In the preparation on the basis of pure PAA, add Tetraethyl orthosilicate (TEOS), the sol - gel (Sol-gel) reaction, by thermal imidization process, prepared with different silica (SiO2) content polyimide / silica (PI/SiO2) composite films. Different silica (SiO2) content of concentrated acid with water and processing water without catalyst under the conditions of acid catalysis, since the three systems into PI/SiO2/H2O, PI/SiO2/H2O/H2SO4 and PI/SiO2, hydrolysis were compared characteristics of the film. Then, using ultraviolet (UV-vis) spectroscopy, infrared (IR) spectroscopy, thermal gravimetric analysis (TGA) tests were studied structure and properties of these materials. The results show that: with the increase of SiO2 content, PI/SiO2decreased transparency, acid water system withouttransparency,higher than the water plus acid system.
Key words: polyimide; silica; sol - gel; Nanocomposites
辽宁科技大学本科生论文 第III页
目 录
摘 要 ........................................................................................................................................ I Abstract ....................................................................................................................................... II 目 录......................................................................................................................................... III 1绪 论....................................................................................................................................... 1
1.1 研究背景及意义 ........................................................................................................... 1 1.2 聚酰亚胺的研究 ........................................................................................................... 2
1.2.1 聚酰亚胺薄膜国内外概况................................. 2 1.2.2 聚酰胺酸的合成机理..................................... 4 1.2.3 聚酰亚胺的合成方法..................................... 4 1.2.4 聚酰亚胺的性能......................................... 5 1.2.5 聚酰亚胺纳米复合材料薄膜............................... 6 1.2.6 聚酰亚胺复合材料薄膜制备方法 ............................................................. 7 1.3 论文研究内容 ............................................................................................................... 9
2 实验部分 .............................................................................................................................. 10
2.1 试剂与药品 .................................................................................................................. 10 2.2 仪器装置 ...................................................................................................................... 11
2.2.1 实验所用仪器和设备.................................... 11 2.2.2 附属设备 ......................................................................................................... 11 2.3 聚酰亚胺的合成 ......................................................................................................... 11
2.3.1反应原理 .............................................. 11 2.3.2 聚酰亚胺的合成 ........................................................................................... 12 2.4 PI膜的酰亚胺化过程 ................................................................................................ 13 2.5 聚酰亚胺/二氧化硅纳米复合材料膜的合成 ..................................................... 13
2.5.1合成方法 .............................................. 13 2.5.2 反应原理.............................................. 14 2.5.3 聚酰亚胺/二氧化硅的合成 ....................................................................... 14 2.6 实验配方表 .................................................................................................................. 15
3 实验结果与讨论 .............................................................................................................. 17
3.1 红外光谱 ...................................................................................................................... 17
1）PI/SiO2体系 ............................................. 17 2.）PI/SiO2/H2O（H2SO4)体系................................. 17 3.）PI/SiO2/H2O体系 ............................................................................................ 18 3.2脱水率的计算 .............................................................................................................. 19 3.3 紫外光谱 ...................................................................................................................... 20 3.3 溶解性测试 .............................................................................................................. 23
辽宁科技大学本科生论文 第IV页
3.3.1 测试方法 ........................................................................................................... 23 3.3.2 实验结果 ...................................................................................................... 23 3.4 核磁共振 .................................................................................. 错误！未定义书签。
结 论 ................................................................................................................................... 25 致 谢 ................................................................................................................................... 26 参考文献 ................................................................................................................................... 27