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材料研究学报  2016, Vol. 30 Issue (11): 868-874    DOI: 10.11901/1005.3093.2016.098
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氯化银光引发聚合制备单分散聚苯乙烯微球
杨莹,赵岩,颜雨坤,张劲松
中国科学院金属研究所 沈阳 110016
AgCl Nano-cubics Used as Photoinitiator for Polymerizing Monodispersed Polystyrene Microspheres
Ying YANG,Yan ZHAO,Yukun YAN,Jinsong ZHANG
Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China
引用本文:

杨莹,赵岩,颜雨坤,张劲松. 氯化银光引发聚合制备单分散聚苯乙烯微球[J]. 材料研究学报, 2016, 30(11): 868-874.
Ying YANG, Yan ZHAO, Yukun YAN, Jinsong ZHANG. AgCl Nano-cubics Used as Photoinitiator for Polymerizing Monodispersed Polystyrene Microspheres[J]. Chinese Journal of Materials Research, 2016, 30(11): 868-874.

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摘要: 

以氯化银颗粒为光引发剂, 以聚乙烯吡咯烷酮(PVP)为分散稳定剂, 在紫外光辐照下引发苯乙烯单体聚合制备了单分散的聚苯乙烯微球。用扫描电子显微镜(SEM)、傅里叶红外光谱(FT-IR)等手段对光诱导聚合产物进行了表征, 用差示扫描量热仪(DSC)测试了聚苯乙烯微球的玻璃化转变温度。反应动力学研究表明, 这种聚合反应符合一级反应动力学特征; 反应机理研究证明, 该聚合反应属于自由基聚合, 乙氧基自由基(CH3CH2O)为引发聚合反应的活性基团。在紫外光的照射下, 这种氯化银立方体颗粒具有一定的稳定性。

关键词 有机高分子材料氯化银光引发聚苯乙烯微球聚合    
Abstract

Mono-dispersed polystyrene microspheres were prepare by UV irradiation assisted polymerization of styrene monomer with AgCl nano-cubic particles as photoinitiator and polyvinylpyrrolidone (PVP) as dispersion stabilizer. The morphology, molecular structure and glass transition temperature of the polymers were characterized by SEM, FT-IR and DSC respectively. From the polymerization dynamics, it follows that the photopolymerization process was a first order reaction. The photopolymerization reaction could be identified as a kind of free radical polymerization, while CH3CH2O was the active group in the photopolymerization. Besides, AgCl nano-cubic particles were stable under UV irradiation.

Key wordsorganic polymer materials    AgCl    photoinitiate    polystyrene microspheres    polymerize
收稿日期: 2016-02-16     
图1  AgCl颗粒的SEM形貌和粒径分布曲线
图2  36W紫外灯辐照不同时间AgCl纳米颗粒溶胶的数码照片
图3  紫外光照10 min氯化银纳米颗粒的SEM照片
图4  紫外光照射后AgCl的XRD谱图
图5  光引发聚合制备的聚苯乙烯微球的SEM照片和粒径分布柱状图
图6  聚苯乙烯的红外光谱
图7  光引发聚合和普通热引发聚合的聚苯乙烯微球的DSC曲线
Reaction time/h mn / Da mw / Da PDI
1 10629 14657 1.379
2 25584 39864 1.558
3 33600 50687 1.509
4 46278 72795 1.573
5 52778 81384 1.542
6 96604 154759 1.602
表1  聚苯乙烯不同反应时间的GPC分子量
图8  苯乙烯的光聚合反应动力学曲线
Runa Adding AgCl particles or not Salicylic acid/g Degassing/ Time(min) α(%)b Mnc(Da) Polydispersity index(Mw/ Mn)
1 Yes - N2/25 26.06 33600 1.509
2 Yes 0.0054 N2/25 25.97 32945 1.537
3 Yes - O2/25 - - -
4 No - N2/25 - - -
表2  AgCl紫外光引发苯乙烯聚合反应
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