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采用一种简单易行的方法制备了氨基功能化的聚苯乙烯纳米粒子.首先,采用4-乙烯基苄氯与1,3-丙二胺置换反应制备了含有氨基功能基团的可聚合单体N-(3-氨基丙基)对乙烯基苄基亚胺(CVPD).然后,采用乳液聚合,以苯乙烯(St)和CVPD为共聚单体,水溶性的4-(2-羟乙氧基)苯基-(2-羟基-2-丙基)酮(Irgacure 2959)为光引发剂,十六烷基三甲基溴化铵(CTAB)为乳化剂,经紫外光辐照引发,合成了P(St-co-CVPD)二元共聚物的纳米胶乳.体系的乳化剂用量仅为体系总质量的0.1 wt%~0.8 wt%,远小于常用来制备纳米粒子的微乳液体系的乳化剂用量.用透射电子显微镜(TEM)和激光粒度分析仪(DLS)表征了P(St-co-CVPD)纳米粒子的粒径和粒径分布.用红外光谱(FTIR)和核磁共振(NMR)证明了P(St-co-CVPD)纳米粒子上氨基的存在,并通过茚三酮显色反应定量检测了氨基含量.分别研究了单体配比,引发剂浓度,乳化剂用量以及紫外光强度对反应体系的影响.实验结果表明,产物粒子尺寸为30~600 nm,氨基通过共价键连接在粒子上,其含量为1.2×10-5~1.6×10-4 mol/g.该乳液体系聚合反应速率较快,单体转化率在60 min内即可达到80%.所得粒子的氨基含量可以通过单体配比进行调节.粒子尺寸可通过单体配比,引发剂浓度,乳化剂用量以及紫外光强度进行调节.
Amino-functionalized polystyrene nanoparticles were prepared by a simple and easy method.Firstly, the polymerizable functional groups containing amino functional groups were prepared by displacement reaction of 4-vinylbenzyl chloride and 1,3-propanediamine N- (3-aminopropyl) p-vinylbenzylimine (CVPD) .Then, using emulsion polymerization, styrene (St) and CVPD as comonomers, water-soluble 4- Oxy) phenyl- (2-hydroxy-2-propyl) ketone (Irgacure 2959) as photoinitiator and cetyltrimethylammonium bromide (CTAB) as emulsifier, The nano-latexes of P (St-co-CVPD) binary copolymer were synthesized.The emulsifier dosage was only 0.1 wt% ~ 0.8 wt% of the total mass of the system, much less than that of the microemulsion system used to prepare nanoparticles The particle size and particle size distribution of P (St-co-CVPD) nanoparticles were characterized by transmission electron microscopy (TEM) and laser particle size analyzer (DLS) .The results of Fourier transform infrared spectroscopy (FTIR) and nuclear magnetic resonance (NMR) The presence of amino groups on P (St-co-CVPD) nanoparticles was demonstrated, and the amino group content was quantitatively determined by the colorimetric reaction of ninhydrin.The monomer ratio, initiator concentration, emulsifier dosage and The effect of external light intensity on the reaction system was studied.The experimental results showed that the particle size of the product was 30-600 nm and the amino group was covalently attached to the particle with the content of 1.2 × 10-5-1.6 × 10-4 mol / g. The emulsion polymerization rate is faster, the monomer conversion can reach 80% within 60 min. The amino group content of the particles can be adjusted through the monomer ratio.Particle size can be determined by the monomer ratio, initiator concentration, Emulsifier dosage and UV intensity to be adjusted.