富炔高分子/纳米钯复合吸氢材料的制备及表征

Preparation and characterization of Pd nanoparticles/alkynyl-riched composite hydrogen material

以聚乙烯醇(PVA)为基体,分别通过醚化反应和氨基甲酸酯化反应在PVA高分子链上引入炔基形成富炔高分子,用红外、核磁共振法对富炔高分子的分子结构及接枝度进行表征。利用化学还原法制备出富炔高分子负载纳米钯的复合吸氢材料,采用透射电镜(TEM)对复合材料的形貌及微观结构进行表征,确定纳米钯的形貌、粒径分布以及其在富炔高分子基体中的分散情况。结果表明,溴丙炔醚化改性PVA因溶解性问题导致纳米钯分散性不好、团聚现象严重;而炔丙胺氨基甲酸酯化改性PVA负载的纳米钯粒径均一,分散性良好,为下一步吸氢性能的研究打下基础。

Poly（vinyl alcohol）（PVA）polymer material was used as substrate.Novel PVA functionlized with pendant acetylene groups were respectively prepared by etherification and carbamate esterification reactions to PVA,which formed alkynyl-riched polymers.The structure and degree of substitution of the resulting alkynyl-riched polymers were characterized by means of infrared spectroscopy and nuclear magnetic resonance spectroscopy.Pd nanoparticles/alkynylriched polymer composites were synthesized in the course of in stiu reduction reaction.Transmission electron microscopy（TEM）was applied to characterize the shape and microstructure of composites in order to ensure morphology,particle size distribution and dispersion in polymer matrix of palladium nanoparticles.Results showed that the solubility of propargyl bromide-modified PVA can lead to poor dispersion and undesired agglomeration,and Pd nanoparticles that were encapsulated with propargylamine-modified PVA had size uniformity and good dispersion.Therefore,the method will lay the foundation for the next step research of absorption hydrogen performance.