疏水性聚酰亚胺增强SiO2气凝胶复合材料的制备与表征

Preparation and characterization of hydrophobic polyimide reinforced SiO2 aerogel composites

  • 摘要: 采用化学交联、溶胶-凝胶和表面改性的方法,制得疏水性聚酰亚胺(PI)增强SiO2气凝胶复合材料。以均苯四甲酸二酐(PMDA)和4’,4’-二氨基二苯醚(ODA)为聚合单体,3-氨丙基-三己氧基硅烷(APTES)为封端剂,合成APTES封端的聚酰亚胺,与正硅酸乙酯(TEOS)混合形成前驱体。采用酸碱两步催化凝胶、湿凝胶依次进行表面疏水改性、溶液置换及CO2超临界干燥,得到聚酰亚胺增强SiO2气凝胶复合材料样品。利用FTIR、SEM、比表面积测试仪、万能材料试验机、接触角分析仪等表征样品的化学组成、微观形貌、孔结构、力学性能及疏水性能等。结果表明:PI质量分数为6wt%的样品密度为0.124 g/cm3,比表面积为724 m2/g,平均孔径尺寸为14 nm,接触角为134°,抗压强度为0.295 MPa。20wt%含量的PI增强SiO2气凝胶样品抗压强度为0.556 MPa。

     

    Abstract: The hydrophobic polyimide (PI) reinforced silica aerogel composite was prepared by the methods of chemical cross-linking, sol-gel and surface modification. The 3-aminopropyltriethoxysilane (APTES) end capped polyimide synthesized from pyromelliticdianhydride (PMDA), 4,4'-oxydianiline (ODA) as the polymer monomers and APTES as the blocking agent, was mixed with tetraethoxysilane (TEOS) to form the precursor. The PI reinforced SiO2 aerogel composite samples were obtained via a technological process of acid/base two-step catalytic, surface hydrophobic modification, solvent exchange and carbon dioxide supercritical fluid drying. The chemical composition, micro-morphology, porous structure, mechanical and hydrophobic properties were studied by the FTIR, SEM, specific surface analyzer, universal testing machine and contact angle analyzer. The results show that the density of PI reinforced SiO2 aerogel composite with 6wt% PI mass fraction is 0.124 g/cm3, the specific surface area is 724 m2/g, the average pore size is 14 nm, the water contact angle is 134° and the compressive strength is 0.295 MPa. When the PI mass fraction is up to 20wt%, the compressive strength of the sample is 0.556 MPa.

     

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