An effective cross-linking of polymer layer on monodisperse, poly(maleic anhydride-styrene)-modified colloidal silica particles and properties of the composite

Summary  The cross-linkings of the surface polymer layer on mono disperse, poly(maleic anhydride-styrene)-modified silica particles by the reaction with diisocyanate were studied. The extent of cross-linking was estimated by the weight decrease by immersing the particles in the buffer solution of pH 2.0, 4.0 and 9.0 at a room temperature for 24 h. The reaction of the polymer-modified silica with 1,6-diisocyanatohexane afforded relatively stable composite particles which lost less than 5 wt% of the polymer in aqueous solution in the pH range 2.0–9.0. The diisocyanate was a preferable cross-linker to 2,4-diisocyanatotoluene in terms of stability in acidic or basic aqueous solution. The flexibility of the cross-linker molecule possibly plays an important role in the cross-linking reaction. The carboxyl and amino groups were formed by treating the cross-linked composite particles with diluted HCl solution; 5–6 and 0.5–1.1 μmol g^-1, respectively. The cross-linked composite particles exhibited the characteristic property of ζ-potential, −44 to −47 mV and −102 to −107 mV in a neutral aqueous solution and ethanol, respectively. Received: 26 May 1997 Accepted: 4 August 1997     

Preparation of Immobilized Metal Affinity Chromatographic Packings Based on Monodisperse Hydrophilic Non‐porous Beads and Their Application

Three hydrophilic immobilized metal affinity chromatographic packings for HPLC have been synthesized by chemical modification of 3.0 µm monodisperse non‐porous poly(glycidyl methacrylate‐co‐ethylenedimethacrylate) (P_GMA/EDMA) beads. The retention behavior of proteins on the metal ion chelated columns loaded with copper(II), nickel(II) and zin(II) ion was studied. The effect of pH on the protein retention was investigated on both the naked and metal ion chelated columns in the range from 4.0 to 9.0. Four proteins were quickly separated in 3.0 min with linear gradient elution at a flow rate of 3.0 mL/min by using the synthesized Ni²⁺‐IDA (iminodiacetic acid) packings. The separation time was shorter than other immobilized metal affinity chromatography reported in the literature. Purification of lysozyme from egg white and trypsin on the commercially available trypsin was performed on the naked‐IDA and Cu²⁺‐IDA columns, respectively. The purities of the purified trypsin and lysozyme were more than 92% and 95%, respectively.     

Production of micron-sized monodispersed composite polymer particles by seeded polymerization utilizing the dynamic swelling method

 In order to develop the seeded polymerization technique utilizing the dynamic swelling method (DSM) proposed by authors for the production of micron-sized mono-dispersed “composite” polymer particles consisting of two kinds of polymers, the seeded polymerization for the dispersion of ethyl methacry-late (EMA)-swollen PS particles prepared utilizing DSM was carried out. Monodispersed PS/poly(ethyl methacrylate) (PEMA) composite particles having 7 μm in diameter were produced by the addition of NaCl to lower the solubility of EMA in medium and by the addition of CuCl₂ as a water-soluble inhibitor to depress the by-production of submicron-sized PEMA particles. Received: 16 July 1996 Accepted: 10 October 1996     

Controlled synthesis and self-assembly of highly monodisperse Ag and Ag(2)S nanocrystals

A facile method to control the synthesis and self‐assembly of monodisperse Ag and Ag₂S nanocrystals with a narrow‐size distribution is described. Uniform Ag nanoparticles of less than 4 nm were obtained by thermolysis of Ag–oleate complexes in the presence of oleic acid and dodecylamine, and monodisperse Ag nanoparticles of less than 10 nm were also prepared in one step by using dodecylamine and oleic acid as capping agents. Moreover, the surface‐enhanced Raman scattering (SERS) properties of the Ag substrates have also been investigated. It is worth mentioning that these Ag nanoparticles and assemblies show great differences in the SERS activities of Rhodamine B dye. In addition, the superlattices of Ag₂S nanocrystals were synthesized with Ag–oleate complexes, alkanethiol, and sulfur as the reactants. The resulting highly monodisperse nanocrystals can easily self‐assemble into interesting superstructures in the solution phase without any additional assembly steps. This method may be extended to the size‐controlled preparation and assembly of many other noble‐metal and transition‐metal chalcogenide nanoparticles. These results will aid the study of the physicochemical properties of the superlattice assemblies and construction of functional macroscopic architectures or devices.     

单分散聚苯乙烯微球的制备及影响因素研究

以聚乙烯吡咯烷酮为分散剂，无水乙醇为反应介质，偶氮二异丁腈为引发剂，采用分散聚合工艺，通过优化反应条件，制备出了粒径为5μm单分散（分散系数≤5％）聚苯乙烯微球。所制备的聚苯乙烯微球标准偏差δ＝0．16μm，分散系数ε＝0．02，且具有良好的球形度，表面非常光滑，无破损，无缺损。对影响单分散聚苯乙烯微球的因素进行了研究，结果表明：随着分散稳定剂用量的增加，聚苯乙烯微球的粒径减小；随着单体和引发剂用量的增加，聚苯乙烯微球的粒径增大。分散稳定剂和单体用量是影响聚苯乙烯微球粒径分布的两个主要因素。     

Studies on Monodispersed Microspheres of Zinc Sulfide Doped with Mn^2＋

In this paper,zinc acetate,manganese acetate and thiacetamide are used as raw materials to successfully synthesize monodispersed ZnS:Mn2+ microspheres by using hydrothermal method and taking P123 surfactant as a template. The products were characterized by XRD,STEM,FT-IR and N2 adsorption-desorption. And the results show that the diameter of this microsphere is 1.0 μm or so,which is larger than that of ZnS microsphere without Mn2+ doping,and it has monodispersion,smooth surface and uniform size. The doping of Mn2+ does not obviously change the structure of monodispersed ZnS microsphere. The photoluminescence peak lies in a wide band ranging from 450 to 650 nm,and the microspheres emit orange light; with the increase of Mn2+ concentration,fluorescence intensity of ZnS:Mn2+ microsphere changes,and when the mole ratio of Mn2+:Zn2+ is 0.3:1,the fluorescence intensity is the strongest.     

nFe3+/nSr2+和nOH-/nNO3-对锶铁氧体纳米片结构及磁性能的影响

采用改进的水热法成功合成了单分散的纯相锶铁氧体纳米片。借助DLS、XRD、FTIR、SEM、EDS和VSM等分析测试手段对SrFe₁₂O₁₉铁氧体粉体的粒度、结构、形貌和磁性能进行表征。研究结果表明,在240℃保温5 h,物质的量之比n_Fe³⁺/n_Sr²⁺(R_F/S)和n_OH^-/n_NO3^-(R_O/N)分别为5和2时,所得产物为单分散的纯相六角SrFe₁₂O₁₉铁氧体纳米片。随着R_F/S和R_O/N的变化,合成样品中有少量SrCO₃和Fe₂O₃杂相存在,这主要与反应条件和离子比例有关。磁性能测试结果显示,所得纯相的六角SrF₁₂O₁₉铁氧体纳米片具有优异的磁性能,其饱和磁化强度和矫顽力分别达到60.91 emu·g^-1和94.83 kA·m^-1,使其在医疗、催化和生物等高技术领域具有潜在的应用。     

新型L-羟脯氨酸聚合物键合手性固定相的制备及对手性化合物的拆分

以单分散亲水性交联聚甲基丙烯酸环氧丙酯-甲基丙烯酸乙二醇双酯(PGMA/EDMA)树脂为载体,制备新型L-羟脯氨酸聚合物键合高效手性配体交换固定相。该固定相在配体交换分离模式下,以0.2mol/LNaAc和0.1mmol/LCu(Ac)2水溶液(pH5.2)为流动相,柱温为30℃～50℃,对衍生和非衍生的D,L-氨基酸和α-羟基酸等9种手性化合物进行了高效液相色谱拆分。详细考察了流动相pH值、温度、流速和进样量对手性分离的影响,选择了合适的色谱分离条件。结果表明,所拆分的9种手性化合物,有5种手性化合物能得到基线分离,最好的分离因子α=2.32。     

Synthesis and characterization of polymethacrylates containing conjugated oligo(phenylene ethynylene)s as side chains

In order to form suitable systems designed for resonance energy transfer, a series of monodisperse methacrylate‐based monomers containing rigid π‐conjugated oligo(phenylene ethynylenes) with different sizes of the conjugated systems ( M1 – M3 ), and therefore different optoelectronic properties, were synthesized and subsequently polymerized using the reversible addition–fragmentation chain transfer polymerization technique ( P1 – P3 ). In addition, these oligomers were also copolymerized with methyl methacrylate. The obtained polymers were characterized by ¹H NMR spectroscopy, size exclusion chromatography, and analytical ultracentrifugation. The photophysical properties of the polymers were studied by UV–vis absorption and emission spectroscopy in diluted solutions as well as in thin films and compared to the photophysics of the corresponding monomers. Thereby, changes going from monomeric to polymeric systems could be detected in fluorescence quantum yields and lifetimes pointing to energy trapping, e.g., energy transfer. Donor–acceptor copolymers containing different numbers of monomeric units within the side chain exhibit differences in the emission spectra, indicating that energy trapping in polymers is very sensitive to structural properties such as the chain length. UV–vis absorption spectroscopy as well as time‐resolved lifetime studies indicate intrapolymer and interpolymer energy transfer. © 2012 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2012