单分散窄分布聚苯乙烯微球的制备研究

以苯乙烯为单体,聚乙烯基吡咯烷酮(PVP)为分散剂,偶氮二异丁腈(AIBN)为引发剂,甲醇为分散介质,利用分散聚合法制备了微米级单分散聚苯乙烯微球。通过傅立叶红外分析(FT-IR),扫描电子显微镜(SEM),激光粒度分析(LPS)等方法对微球进行测试表征。研究了PVP用量对微球产物的影响。结果表明:单体的转化率随PVP用量的增加而增大,PS微球的粒径随着PVP用量的增大而减小,其粒径分布先变窄后变宽。当PVP用量为1.5%时微球的粒径分布最窄,单分散性最好。改变PVP用量可以得到不同粒径的PS微球。     

分散聚合法制备亚微米级单分散聚苯乙烯微球

以醇和水的混合液为分散介质,聚乙烯基吡咯烷酮（PVP）为分散剂、偶氮二异丁腈（AIBN）为引发剂,利用分散聚合法制备亚微米级的单分散聚苯乙烯（PS）微球。分别讨论分散剂的用量以及分散介质的溶解度参数对PS微球粒径的影响。结果表明,当分散介质溶解度参数和单体苯乙烯的溶解度参数越接近时,所制得的PS微球粒径越大,反之越小;随着分散剂PVP量的增加,微球的粒径减小,粒径分布变窄;所制得的聚苯乙烯微球表面光滑,呈均匀的球形。     

种子溶胀法制备单分散交联聚苯乙烯微球

采用分散聚合法制备了聚苯乙烯(PS),并以此作为种子,与溶胀剂和单体、交联剂的混合物经二步溶胀聚合法,制备了单分散交联PS微球.讨论了溶胀剂用量、交联剂用量和单体用量对溶胀微球粒径和粒度分布的影响,以及交联剂用量对溶胀微球形貌的影响.结果表明,当溶胀剂的用量为3 g,交联剂为1 g,单体用量为7 g时可制得平均粒径为6.84 μm且单分散性较好的交联PS微球.     

交联型单分散聚苯乙烯微球的制备

以聚乙烯吡咯烷酮（PVP）为分散剂，偶氮二异丁腈（AIBN）为引发剂，乙醇为分散介质，二乙烯基苯（DVB）为交联剂进行了苯乙烯（St）的分散聚合；讨论了引发剂、交联剂、分散剂、单体用量对聚合物粒径及分布的影响，制备了交联型单分散聚苯乙烯微球。实验表明：当交联剂质量分数达到单体质量分数的1％时，微球依然可以保持良好的单分散性。在聚合体系中引入抗坏血酸，使其与微量的氧结合，有效地提高了微球的均匀度。     

连续法制备单分散聚苯乙烯微球及粒径影响因素的研究

以苯乙烯为单体,偶氮二异丁腈(AIBN)为引发剂,聚乙烯吡咯烷酮(PVP)为分散剂,采用连续分段添加引发剂的方法制备微米级的聚苯乙烯微球。研究了引发剂的添加方式,各组分用量变化对聚苯乙烯微球粒径和粒径分布的影响。结果表明:在反应过程中不断地补加引发剂可以保持活性自由基的生成速率,对聚苯乙烯微球的粒径和粒径分布有着重要的影响。在此基础上,通过改变各组分的用量可以制备出表面光洁,粒径在1.3μm左右的聚苯乙烯微球,且单分散性良好,单分散系数在1.02左右。     

无皂乳液聚合法制备亚微米级单分散聚苯乙烯微球

采用无皂乳液聚合法制备了亚微米级聚苯乙烯(PS)微球,考察了苯乙烯(St)单体浓度、引发剂过硫酸钾(K2S2O8)浓度、离子强度(氯化钠浓度)与PS微球粒径及其分布的关系。然后通过加入微量乳化剂或β-环糊精对无皂乳液聚合法进行改进,研究了改进效果。结果表明,PS微球的粒径随St单体浓度和氯化钠浓度的增加而增加、随K2S2O8浓度的增加而减小,通过调节这3种原料的浓度,可制得粒径在450~1000 nm且单分散系数小于0.08的PS微球,但产品收率较低,仅为30%左右。在相同的合成条件下,加入微量乳化剂可制得粒径在100~350 nm且单分散系数小于0.05的PS微球,产品收率提高到75%左右;加入微量β-环糊精可制得粒径在300 nm左右且单分散系数小于0.08的PS微球,产品收率可达80%且反应时间大幅缩短,由原来的12 h缩减到5 h。     

含氟聚苯乙烯微球的制备及其疏水性能研究

以苯乙烯(St)和含氟单体(G04)为原料、聚乙烯吡咯烷酮(PVP)为分散剂和乙醇/水为混合溶剂,采用分散聚合法制备出PS-F(含氟聚苯乙烯)微球;然后以苯丙乳液提供的附着力、PS-F微球提供的疏水性能,制备PS-F疏水涂层。结果表明:制备PS-F微球的最佳工艺条件是m(总单体)=m(St+含氟单体)=20 g且m(St):m(含氟单体)=18:2、w(AIBN)=1.5%、w(PVP)=7.5%、V(乙醇)=108 mL、V(H_2O)=72mL、反应温度70℃和反应时间10 h,此时PS-F微球的粒径为0.4～1.0μm;当w(PS-F微球)=60%时,疏水涂层的水接触角为130。左右;含氟单体含量和苯丙乳液含量对水接触角的影响不大,涂层疏水性能主要与PS-F微球大小、涂层表面粗糙度有关。     

单分散微米级PMMA微球的制备

以聚乙烯吡咯烷酮(PVP)为分散剂,乙醇和水为反应介质,偶氮二异丁腈为引发剂,甲基丙烯酸甲酯(MMA)为单体,采用分散聚合工艺,制备了单分散微米级PMMA微球。研究了乙醇/水介质的配比、反应温度、分散剂用量、单体用量、引发剂用量对PMMA微球粒径和粒径分布的影响。结果表明,PMMA微球粒径随乙醇用量的增加先增大后减小;随反应温度的升高先增大后减小,粒径分布先变窄再变宽;随单体用量的增加先增大后减小,随引发剂用量的增加而增大;随PVP用量的增加而减小,粒径分布先变窄再变宽。     

分散聚合法制备单分散聚苯乙烯微球

用分散聚合法,在乙醇/水介质中,以苯乙烯为单体,偶氮二异丁腈为引发剂,聚乙烯吡咯烷酮为分散剂制备了聚苯乙烯(PS)微球。探讨了制备条件对微球形貌、粒径及粒径分布的影响。结果表明,在合适条件下,可以制备粒径在1μm左右,粒径分布在1.04~1.08,表面光滑且互不粘连的单分散PS微球。     

异丙醇-水介质中微米级单分散聚(苯乙烯-甲基丙烯酸)微球的制备

以苯乙烯和甲基丙烯酸为单体、PVP为分散剂,AIBN为引发剂,在异丙醇-水介质中,用分散聚合方法制备了微米级单分散的聚(苯乙烯-甲基丙烯酸)[P(St-MAA)]微球。结果表明,采用反应初期低温、中后期升温的聚合工艺可制得单分散的聚合物微球,并提高聚合反应的速率和转化率。P(St-MAA)微球的粒径及其分布可通过改变介质组成来控制。分散介质中异丙醇质量分数降低,聚合反应速率增大,转化率升高,微球的粒径减小。当分散介质中异丙醇的质量分数降低到60％时,聚合反应中有凝胶生成,粒径分布呈多分散性。     

Uniform Polystyrene Particles by Dispersion Polymerization in Different Dispersion Medium

Using PVP K-30 as steric stabilizer and AIBN as initiator, uniform polystyrene (PS) particles were prepared by dispersion polymerization of styrene in ethanol/water and isopropanol/ water media. The effects of initiator and stabilizer concentration, alcohol/water volume ratio on the average sizes and size range of PS particles were investigated. Unifrom PS particles in the size range of 0.7-1.7 μm were obtained. The results showed that higher stabilizer concentration led to PS particles with smaller average sizes, and higher initiator concentration caused greater average particle sizes. It was also found that the average sizes reduced and size ranges became narrow as the polarity (solubility parameter) of dispersion medium employed was increased.     

反应体系组成对纳米SiO2/PS复合粒子粒径及分布的影响

研究了在纳米SiO2粒子表面的苯乙烯原位聚合反应中,反应体系的组成(单体、引发剂、稳定剂及纳米SiO2粒子用量)对纳米SiO2/PS复合粒子的形态、粒径大小及分布的影响。结果表明,当纳米SiO2粒子与单体质量比为5%,苯乙烯质量分数为25%,引发剂及稳定剂用量分别为单体用量(质量比)的0.15%和1.5%时,制备出的纳米SiO2/PS复合粒子呈球形,表面光滑无明显缺陷,颗粒之间分散性很好,粒径为0.923μm,分散系数为0.108。     

Preparation,characterization, and drug-release properties of PEG-DA-based copolymer hydrogel microspheres

The research was to design a carrier used in tissue engineering and drug-release system. In this article, a new dispersion polymerization system without organic solvent was described to prepare poly(ethylene glycol) diacrylate/2-hydroxyethyl methacrylate (PEG-DA/HEMA) copolymer hydrogel microspheres as carrier, which introduced chitosan (CS) as reaction medium and costabilizer, polyvinylpyrrolidone (PVP) as steric stabilizer and benzoy peroxide (BPO) as initiator. The effects of mass ratios of monomers, concentration of stabilizer and initiator on partilcle size and polydispersity index (PDI) of microspheres were investigated. Furthermore, bovine serum albumin (BSA) as protein model, the composition of copolymer, size, and polydispersity index of microspheres were employed to study the amount and released ratio of loaded BSA in this article. The results showed that hydrogel microspheres with 3.26 ± 0.24 μm in particle size and 1.03 ± 0.008 in PDI, obtained with mass ratios of PEG-DA 60/HEMA 40, 2 wt % of stabilizer content and 2 wt % of initiator content (relative to total mass of monomers), had 124.57 ± 3.14 mg/g in the amount of loaded BSA and 59.09 ± 1.43% of released ratio. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Dispersion polymerization of n‐butyl acrylate

The dispersion polymerization of n‐butyl acrylate (BA) was investigated using alcohol/water mixtures as the dispersion medium, 4,4′ ‐azobis‐(4‐cyanopentanoic acid) as the initiator, and polyvinylpyrrolidone (PVP) as the stabilizer. The effects of polymerization parameters, such as the alcohol/water ratio in the medium and the type and concentration of the polymeric stabilizer, on the resulting particle size and size distribution were studied. The final particle size and the stability of the dispersion system were found to be greatly influenced by the type of alcohol used in the mixture; that is, methanol or ethanol, even though the apparent solubility parameters are almost the same for the two types of mixtures. Poly(butyl acrylate) particles with controlled size and size distribution (monodisperse), and gel content were successfully prepared in a 90/10 methanol/water medium. It was found that the particle size decreased with increasing initiator concentration. This is the opposite of what was previously reported in the dispersion polymerizations of styrene and methyl methacrylate. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 84: 2692–2709, 2002     

Preparation of micron‐size monodispersed PS/P(St/MAA) microspheres by seeded dispersion polymerization

Uniform polystyrene (PSt) particles with the size of 1.9 μm were first prepared via dispersion polymerization, and then used as the seeds in a second‐stage dispersion copolymerization of styrene (St) and methacrylic acid (MAA) to produce carboxyl‐carrying microspheres. The PSt seed particles were swollen by monomer mixture of St and MAA, including an oil‐soluble initiator 2,2′‐azobisiso‐butyronitrile (AIBN), before polymerization. Finally, uniform PS/P(St/MAA) (polydispersity index, PDI = 1.02) microspheres with the size of 2.2 μm were obtained. The average particle size and size distribution of the final microspheres were investigated. MAA contents between 54 and 97 mg/g were detected from the PS/P(St/MAA) particles produced under different conditions. Dispersion medium has great influence on the kinetics of polymerization, due to its effect on the partitioning of monomers, solvents, and initiator in the particle phase, probably as well as on the conformation of the dispersion agent on the surface of the particles. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 99: 3586–3591, 2006     

Monosize polystyrene latices carrying functional groups on their surfaces

In this study, monosized polystyrene (PS) latices were prepared by dispersion polymerization of styrene in isopropanol-water media using poly(acrylic acid) (PAA) as a steric stabilizer and 2,2′-azobisizobutyronitrile (AIBN) as an initiator. The effects of initiator and stabilizer concentrations, alcohol/water and monomer/dispersion medium ratio on the polymerization kinetics, and the size and monodispersity of PS latices were experimented with in a stirred reactor system. Monosize PS beads in the size range of 1.0–3.0 μm were obtained. The PS latex obtained in the first step having a diameter of 2.3 μm were used as the seed latex, and styrene/acrylate monomers, acrylic acid (AA), 2-hydroxyethyl methacrylate (HEMA), and dimethylaminoethyl methacrylate (DMAEMA) were copolymerized onto the PS latex particles. The incorporation of functional groups to the surface and bulk structure of PS was confirmed by IR, FTIR, XPS, and zeta potential measurements. © 1994 John Wiley & Sons, Inc.     

羧基聚苯乙烯微球的单分散性制备及表征

文章通过分散聚合法,以苯乙烯（St）为聚合单体,聚乙烯吡咯烷酮（PVP）为稳定剂,偶氮二异丁腈（AIBN）为引发剂,乙醇和水作为分散介质,合成微米级聚苯乙烯微球,并以此微球为种子,利用种子修饰法进一步合成羧基聚苯乙烯微球,并对合成的羧基微球单分散性、表面形貌及表面羧基密度进行表征。结果表明,在合成的聚苯乙烯微球表面成功连接上羧基基团,微球具有较高的羧基密度,并且保持良好的单分散性,适合下一步在其表面进行化学与生物活化以制备液相芯片的敏感元件。     

分散聚合法合成含有环氧基的无孔超顺磁性微球及其表征

Non-porous superparamagnetic polymer microspheres with epoxy groups were prepared by dispersion polymerization of glycidyl methacrylate (GMA) in the presence of magnetic iron oxide (Fe3O4) nanoparticles coated with oleic acid. The polymerization was carried out in the ethanol/water medium using polyvinylpyrrolidone (PVP) and 2,2'-azobisisobutyronitrile (AIBN) as stabilizer and initiator, respectively. The magnetic microspheres obtained were characterized with scanning electron microscopy (SEM), vibrating sample magnetometry (VSM) and Fourier transform infrared spectroscopy (FTIR). The results showed that the magnetic microspheres had an average size of 1μm with superparamagnetic characteristics. The saturation magnetization was found to be 4.5emu·g-1. There was abundance of epoxy groups with density of 0.028 mmol·g-1 in microspheres. The magnetic PGMA microspheres have extensive potential uses in magnetic bioseparation and biotechnology.