以4-乙烯基吡啶为单体,N,N’-亚甲基双丙烯酰胺为交联剂,在超临界二氧化碳(scCO2)中,通过沉淀聚合方法制备了交联聚(4-乙烯基吡啶)的干燥粉末。考察了反应体系的引发剂浓度、交联剂浓度、反应压力、反应时间等因素对聚合反应的影响。通过红外光谱(FT-IR)和扫描电镜(SEM)对聚合物组成及形貌进行了表征。实验表明,反应压力为14MPa,温度为70℃时,在适当交联剂用量下,可获得粒径约为0.5μm-1μm的干燥粉末,所得聚合物的产率大于90%。
Cross-linked poly (4-vinylpyridine) (P4-VP) and copolymers were synthesized in supercritical carbon dioxide(scCO2). The slight yellow, dry, fine powders were obtained directly from precipitation polymerization of 4- vinylpyridine (4-VP) in scCO2 with N, N/-methylenebisaerylarnide as the cross-linker. The effects of the reaction pressure, cross-linker ratio, initiator concentration on the yield and morphology of the resulting polymer were investigated by FT-IR and SEM measurements. It is found that under the condition of 14 MPa and 70 ℃, the cross- linked microparticles with the diameter of 0.5/μm-1 μm are generated in scCO2, with the yield of 92 %.
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