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无皂乳液法制备聚苯乙烯荧光微球
摘 要
传统的高分子聚合物荧光微球的制备方法有:乳液聚合法、分散聚合法、悬浮聚合法等。用无皂乳液聚合方法制备的高分子聚合物微球,表面洁净且呈单分散,并可消除乳化剂对环境的污染,成为最新研究的热点。尤其是在涂料及胶粘剂领域。本论文通过无皂乳液聚合法合成了聚苯乙烯荧光微球,证实了无皂乳液聚合法是制备亚微米级单分散聚苯乙烯荧光微球的有效方法。为得到大小可控的单分散荧光微球,本论文研究了无皂乳液聚合体系中聚合单体浓度、引发剂用量、电解质离子强度等因素,对聚苯乙烯荧光微球的粒径、粒径分布的影响,探讨了制备稳定的均分散无皂亚微米级聚苯乙烯荧光微球的条件。利用红外光谱,核磁共振图谱和荧光光谱表征对可聚合的荧光单体,4-甲氧基-N-烯丙基-1,8-萘酰亚胺进行表征。用无皂乳液聚合的方法制苯乙烯和4-甲氧基-N-烯丙基-1,8-萘酰亚胺的聚合物,并用荧光光谱和红外光谱表征。研究结果表明在甲苯中,共聚物荧光光谱激发波长在365nm,发射波长425nm处。
关键词:荧光;无皂乳液聚合;聚苯乙烯;微球
I
Preparation of emulsifier-free emulsion
fluorescent polystyrene microspheres
Abstract
There are several traditional methods to prepare fluorescent microsphere:emulsion polymerization, dispersion polymerization and suspension polymerization. Emulsifier-free emulsion polymerization can be used to prepare surface clean and mono-disperse microspheres. The pollution of the environment from emulsifier is eliminated. Emulsifier-free emulsion polymerization becomes a focus of research. Especially, it is used in the field of adhesives and paint. In this paper, fluorescent polystyrene microspheres were prepared by emulsifier-free emulsion polymerization. The results showed that emulsifier-free emulsion polymerization was an effective method for the preparation of uniform polystyrene microspheres in micron-size. In order to prepare the polystyrene fluorescent microspheres with controllable sizes, the factors on polystyrene microspheres diameter and size distribution have been investigated and discussed, such as monomer concentration, initiator reagent, the ionic strength of electrolyte. The polymerisable fluorescent monomer, 4-ethoxyl-N-allyl-1,8-naphthalimide,was synthesized and characterized using FT-IR spectra,1H NMR and fluorescence spectra. A copolymer of styrene and 4-ethoxyl-N-allyl-1,8-naphthalimide was prepared by emulsifier-free emulsion polymerization and characterized using fluorescence spectra. The fluorescence spectrum of the copolymer displayed excitation at 365 nm and emission at 425 nm in acetone.
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