DPE法制备Poly（St-alt-MAn）微球
发布时间：2018-09-04 21:09
【摘要】： 在1,1-二苯基乙烯(DPE)存在下,以甲基丙烯酸甲酯(MMA)为初始单体,偶氮二异丁腈(AIBN)为引发剂,采用本体聚合法制备出含有DPE片段的大分子引发剂(PMMA-DPE)。然后利用PMMA-DPE为引发剂,以苯乙烯(St)和马来酸酐(MAn)为共聚单体,乙酸异戊酯为溶剂,采用自稳定沉淀聚合法制备了单分散的聚苯乙烯-马来酸酐(Poly (St-alt-MAn))的微球。 采用IR,UV-vis紫外光谱,1H NMR和GPC对产物的结构进行了分析,并用SEM对聚合物微球的形貌进行了表征。系统地研究了PMMA-DPE的用量、单体浓度、单体配比、温度以及不同反应时间对聚合物相对分子量以及微球的形态、粒径大小及分布的影响。 结果表明,由大分子前躯体PMMA-DPE引发聚合制备出的聚苯乙烯-马来酸酐的微球平均粒径在378-776 nm左右。相对于自引发聚合方法制备得到的微球,该聚合方法得到的微球具有很好的形貌且均一性较好,分散系数较低。随着PMMA-DPE用量的增加,聚合物的相对分子量减小,产率增大,聚合物微球的粒径减小,而粒径分布系数增加。随着单体浓度增加,相对分子量、转化率以及微球的粒径均增加,但分散系数基本不变。[St]:[MAn](摩尔比)的增加,聚合物的相对分子量增加,转化率和粒径都呈现先增加后减小的规律,粒径分布大致不变。温度升高,聚合物的相对分子量先增大后减小,单体转化率和粒径分散系数增加,粒径减小。加入的溶剂丁酮量加大,聚合物的相对分子量先增大后减小,单体转化率下降,粒径变差。根据不同反应时间下的聚合物的相对分子量、单体转化率、微球的粒径以及粒径分布,提出了微球增长的可能机理。
[Abstract]:Macromolecular initiators (PMMA-DPE) containing DPE fragments were prepared by bulk polymerization with methyl methacrylate (MMA) as initial monomer and azodiisobutyronitrile (AIBN) as initiator in the presence of 1-diphenyl ethylene (DPE). Then the monodisperse polystyrene-maleic anhydride (Poly (St-alt-MAn) microspheres were prepared by self-stable precipitation polymerization using PMMA-DPE as initiator, styrene (St) and maleic anhydride (MAn) as comonomer and isoamyl acetate as solvent. The structure of the product was analyzed by IR,UV-vis 1H NMR and GPC, and the morphology of polymer microspheres was characterized by SEM. The effects of the amount of PMMA-DPE, monomer concentration, monomer ratio, temperature and reaction time on the morphology, particle size and distribution of polymer were studied. The results show that the average particle size of polystyrene-maleic anhydride prepared by macromolecular precursor PMMA-DPE initiation polymerization is about 378-776 nm. Compared with the microspheres prepared by the self-initiated polymerization method, the microspheres obtained by this polymerization method have good morphology, good uniformity and low dispersion coefficient. With the increase of PMMA-DPE content, the relative molecular weight of polymer decreases, the yield increases, the particle size of polymer microspheres decreases and the particle size distribution coefficient increases. With the increase of monomer concentration, the relative molecular weight, conversion rate and particle size of the microspheres increased, but the dispersion coefficient remained unchanged. The relative molecular weight of the polymer increased with the increase of [St]: [MAn] (molar ratio). The conversion rate and particle size increased first and then decreased, and the particle size distribution was almost unchanged. With the increase of temperature the relative molecular weight of the polymer first increases and then decreases while the monomer conversion and particle size dispersion coefficient increase and the particle size decreases. When the amount of butanone was increased, the relative molecular weight of the polymer first increased and then decreased, the monomer conversion decreased and the particle size became worse. According to the relative molecular weight, monomer conversion, particle size and particle size distribution of the polymer at different reaction times, the possible mechanism of the growth of the microspheres was proposed.
【学位授予单位】：北京化工大学
【学位级别】：硕士
【学位授予年份】：2010
【分类号】：O631.3
本文编号：2223346
[Abstract]:Macromolecular initiators (PMMA-DPE) containing DPE fragments were prepared by bulk polymerization with methyl methacrylate (MMA) as initial monomer and azodiisobutyronitrile (AIBN) as initiator in the presence of 1-diphenyl ethylene (DPE). Then the monodisperse polystyrene-maleic anhydride (Poly (St-alt-MAn) microspheres were prepared by self-stable precipitation polymerization using PMMA-DPE as initiator, styrene (St) and maleic anhydride (MAn) as comonomer and isoamyl acetate as solvent. The structure of the product was analyzed by IR,UV-vis 1H NMR and GPC, and the morphology of polymer microspheres was characterized by SEM. The effects of the amount of PMMA-DPE, monomer concentration, monomer ratio, temperature and reaction time on the morphology, particle size and distribution of polymer were studied. The results show that the average particle size of polystyrene-maleic anhydride prepared by macromolecular precursor PMMA-DPE initiation polymerization is about 378-776 nm. Compared with the microspheres prepared by the self-initiated polymerization method, the microspheres obtained by this polymerization method have good morphology, good uniformity and low dispersion coefficient. With the increase of PMMA-DPE content, the relative molecular weight of polymer decreases, the yield increases, the particle size of polymer microspheres decreases and the particle size distribution coefficient increases. With the increase of monomer concentration, the relative molecular weight, conversion rate and particle size of the microspheres increased, but the dispersion coefficient remained unchanged. The relative molecular weight of the polymer increased with the increase of [St]: [MAn] (molar ratio). The conversion rate and particle size increased first and then decreased, and the particle size distribution was almost unchanged. With the increase of temperature the relative molecular weight of the polymer first increases and then decreases while the monomer conversion and particle size dispersion coefficient increase and the particle size decreases. When the amount of butanone was increased, the relative molecular weight of the polymer first increased and then decreased, the monomer conversion decreased and the particle size became worse. According to the relative molecular weight, monomer conversion, particle size and particle size distribution of the polymer at different reaction times, the possible mechanism of the growth of the microspheres was proposed.
【学位授予单位】：北京化工大学
【学位级别】：硕士
【学位授予年份】：2010
【分类号】：O631.3
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