Polyamide 6/silica hybrid materials by a coupled polymerization reaction
Polyamide 6/silica hybrid materials by a coupled polymerization reaction
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DOI：
10.1039/c5py00815h
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发表时间：
2015-01-01
影响因子：
4.6
通讯作者：
Spange, S.
中科院分区：
文献类型：
--
作者：
Kassner, L.;Nagel, K.;Spange, S.
通过1，1 '，1“，1”“-硅烷四基四氮杂环庚烷-2-酮（Si（epsilon-CL）（4））、6-氨基己酸（epsilon-ACA）和ε-己内酰胺（epsilon-CL）三种单体组分的偶联聚合反应，在一个过程中制备了聚酰胺6/SiO2杂化材料。已发现Si（ε-CL）（4）与ε-ACA一起适合作为二氧化硅和PA 6组分的前体单体。精确调节两种组分的摩尔比，以及生产聚酰胺6/SiO2杂化材料的整个方法与ε-己内酰胺的水解开环聚合的组合对于获得具有低可萃取物含量的均匀产物是非常重要的。与ε-ACA相比，已经发现水不适合作为生产均匀分布的二氧化硅的氧源。该过程在商业实验室高压釜中在8巴初始压力下进行。通过固体Si-29和C-13 NMR谱、DSC和FTIR谱以及电子显微镜测量研究了杂化材料的分子结构和形态。
Polyamide 6/SiO2 hybrid materials were produced by a coupled polymerization reaction of three monomeric components namely 1,1',1 '',1 '''-silanetetrayltetrakis-(azepan-2-one) (Si(epsilon-CL)(4)), 6-aminocaproic acid (epsilon-ACA) and epsilon-caprolactam (epsilon-CL) within one process. Si(epsilon-CL)(4) together with epsilon-ACA has been found suitable as a precursor monomer for the silica and PA6 components. The accurate adjustment of the molar ratio of both components, as well as the combination of the overall process for producing the polyamide 6/SiO2 hybrid material with the hydrolytic ring opening polymerization of epsilon-caprolactam is of great importance to achieve homogeneous products with a low extractable content. Water in comparison with epsilon-ACA has been found unsuitable as an oxygen source to produce uniformly distributed silica. The procedure was carried out in a commercial laboratory autoclave at 8 bar initial pressure. The molecular structure and morphology of the hybrid materials have been investigated by solid state Si-29 and C-13 NMR spectroscopy, DSC and FTIR spectroscopy and electron microscopy measurements.