以苯乙烯为主单体,丙烯酸为功能单体,二乙烯基苯(DVB)为交联剂,偶氮二异丁腈为引发剂,乙腈和甲苯为溶剂,采用回流沉淀聚合法合成了单分散羧基化交联聚苯乙烯微球;然后以1,2-二氯乙烷为溶胀剂,二甲氧基甲烷为外交联剂,在三氯化铁的催化下发生傅-克超交联反应,实现微孔化。采用傅里叶变换红外光谱、扫描电子显微镜、激光粒度及Zeta电位、比表面积及孔隙分析对微球结构进行了表征。结果表明,通过实验可以得到具有良好球形形貌和单分散性的交联微孔聚苯乙烯微球;随着丙烯酸含量增加,交联微球的带电量增加;随着DVB含量的增加,实现了微孔化且比表面积呈上升趋势,其中当DVB用量为60%时,其比表面积达到606.06 m^2/g。
The monodisperse crosslinked carboxyl-functionalized polystyrene microspheres were synthesized via reflux precipitation polymerization with styrene as main monomer, acrylic acid as functional monomer, divinylbenzene(DVB) as crosslinker, 2,2-azobis(isobutyronitrile) as initiator and the mixed solvent of acetonitrile and toluene as medium; then the micropores microspheres were achieved through the Friedel-Crafts reaction with 1,2-dichloroethane as sweller, formaldehyde dimethyl acetal as external crosslinker and anhydrous ferric chloride as catalyst. The morphology and structure were characterized by FT-IR, SEM, laser particle size and potential analyzer, specific surface area and porosity analyzer. The results indicate that monodisperse crosslinked carboxyl-functionalized microporous polystyrene microspheres with good spherical morphology can be obtained by experiments; Zeta potential on the surface of microspheres increases with the increasing of acrylic acid; meanwhile, with the increasing of divinylbenzene content, micropores form and BET surface area also increase, the as-prepared microporous microspheres′ BET surface area can be as high as 606.06 m^2/g when the DVB volume fraction is 60%.