磁性聚醋酸乙烯酯微球的制备及表面功能化修饰

在油酸包覆的Fe3O4磁流体存在条件下,以醋酸乙烯酯为聚合单体,二乙烯苯为交联剂,过氧化苯甲酰为引发剂,聚乙烯醇为稳定剂,采用改良悬浮聚合法制备了粒径在数微米之间的磁性聚醋酸乙烯酯微球,对制备的磁性微球进行了表面功能化修饰。利用扫描电镜、振动样品磁强计和Fourier变换红外光谱分别检测了磁性微球的形貌、磁性能以及微球表面修饰的活性功能基团。结果表明:微球大小在1～7μm,平均粒径为3.8μm,粒径分布相对较窄;比饱和磁化强度为15.0emu/g,具有超顺磁性。     

羧基磁性高分子微球的制备和表征

用改进的悬浮聚合法制备了表面含有羧基功能团的聚苯乙烯磁性微球。考察了磁微球的形态与结构 ,测定了磁微球的粒径与磁响应性 ,主要研究了单体 /水、丙烯酸 /单体、反应温度和反应时间对磁性微球形成的影响 ,并对磁性微球的生物吸附活性进行了表征。优化得到了制备具有良好生物吸附活性的羧基磁性微球的最佳实验条件     

表面功能化磁性聚苯乙烯纳米微球的尺寸可控制备

考察了核壳式表面功能化磁性聚苯乙烯纳米微球的可控制备工艺。采用紫外可见吸收光谱、透射电子显微镜、原子力显微镜及在不同溶剂中的分散性实验,对表面羧基化的磁性聚苯乙烯纳米微球的结构与形态进行了表征。结果表明,改变外加晶核Fe2O3纳米颗粒数目,可有效实现磁性聚苯乙烯纳米微球的尺寸可控。     

彩色聚苯乙烯微球的制备

以无机染料和苯乙烯为原料,磷酸三钙(TCP)和聚乙烯醇(PVA)为分散剂,过氧化二苯甲酰为引发剂,通过原位悬浮聚合的方法制备了球度好、有光泽的彩色聚苯乙烯微球。研究了无机染料在苯乙烯中的超声分散时间对分散效果的影响,以及聚合反应过程中分散剂用量、聚合温度、时间对聚合的影响。结果表明:无机染料用量越多,其在苯乙烯中超声分散所需时间越长,分散时间不能小于6 min;较佳聚合条件是分散剂质量比m(TCP):m(PVA)=1:1,采用分段升温反应,先在75℃下反应1 h,然后缓慢升温至85℃反应2 h,最后在95℃下反应0.5 h。通过色差计对彩色聚苯乙烯微球的测试结果表明,随染料添加量的增加,样品的色差变大。     

单分散氢氧化钙/聚苯乙烯微球的制备与表征

以葡萄糖水溶液为反应介质,在氧化钙消化成氢氧化钙的过程中,加入苯乙烯单体和引发剂,采用原位悬浮聚合法成功制备了聚苯乙烯(PS)包覆氢氧化钙[Ca(OH)2]形成Ca(OH)2/PS微球.考察了葡萄糖水溶液、苯乙烯、稳定剂聚乙烯醇以及反应温度对单分散Ca(OH)2/PS微球的粒径及粒子分散系数的影响,得出较佳合成条件.在较佳条件下制备的Ca(OH)2/PS微球平均粒径为30～40 μm,粒子分散系数为0.08～0.10.扫描电镜照片表明,Ca(OH)2/PS具有良好的球形度,表面光滑、无破损.红外光谱表征显示,产物为Ca(OH)2/PS微球.     

多孔性聚苯乙烯磁性微球的制备

以磁流体颗粒为核,采用乳液聚合法合成了聚苯乙烯磁性微球.用该微球作为种子,采用分散聚合法,以乙二醇/水为分散介质,聚乙二醇为分散剂,甲苯为制孔剂,进行二乙烯苯-丙烯酸-苯乙烯三元共聚物的合成,最终合成了粒径大小均匀、具有强磁响应性的多孔聚苯乙烯磁性微球.     

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。     

磁性多孔聚苯乙烯微球的制备

在磁流体存在的情况下,采用改进了的乳液聚合法合成了具有磁核的微米级高分子聚苯乙烯微球。以该微球为种子,采用分散聚合法,以乙二醇／水为分散介质、聚乙二醇为分散剂、甲苯为制孔剂,进行苯乙烯-丙烯酸-二乙烯苯的三元共聚物的合成,最终合成出粒径分布均匀、磁响应性强的磁性多孔聚苯乙烯微球。     

BaFe12O19/聚氨酯磁性复合微球的制备和表征

通过BaFe12O19硅烷偶联剂改性,聚乙二醇1000、甲苯二异氰酸酯在二甲苯溶液中预聚合,预聚物溶液在分散剂聚乙烯吡咯烷酮K30的水溶液中悬浮聚合,三步合成了BaFe12O19/聚氨酯复合微球.用扫描电镜、红外光谱仪、热重-差示扫描同步热分析仪和振动样品磁强计对微球的形貌、结构、玻璃化温度(Tg)和磁性能进行了表征.结果表明:合成的微球以BaFe12O19颗粒为核聚氨酯为壳.表面分布有微孔,微球粒径在400μm左右,粒径大小可通过控制反应条件调节.微球中磁性物质BaFe12O19的含量为11.11%(质量分数),Tg在290 ℃左右,耐热性能好,微球的饱和磁化强度为3.36×103 A/m,矫顽力为3.06×104 A/m.该复合微球是一种有潜在应用价值的新型血管内栓塞材料.     

大粒径磁性高分子微球的合成

本文研究了苯乙烯，丙烯酸等单体在磁性氧化铁的醇／水分散体系中的聚合行为。为了改善磁性氧化铁粒子与苯乙烯单体间的亲合性，加入聚乙二醇作为发散剂和稳定剂，制备出业径为３０－１０００μｍ的具有磁响应性的聚苯乙烯微球。     

Preparation and properties of magnetic polystyrene microspheres

Magnetic polystyrene nanospheres were efficiently prepared by using a new indirect process based on miniemulsion polymerization of styrene. The samples were characterized by X‐ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, transmission electron microscopy (TEM), X‐ray photoelectron spectroscopy (XPS), and vibrating‐sample magnetometry (VSM), respectively. The experimental results clearly show that the 3‐methacryloxypropyltrimethoxy silane was anchored onto the surface of the magnetic particles to form the vinyl end. The size of the magnetic particle is about 6–30 nm. The size of the magnetic particle capped with polystyrene is about 1–2 μm. The magnetic polystyrene spheres exhibit multidomain character, whereas the pure magnetic particles show single domain character. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 3660–3666, 2007     

磁性壳聚糖微球的研究进展

磁性氧化铁纳米粒子（Fe3O4,γ-Fe2O3等）因具有尺寸小、超顺磁性和低毒性等特点,已经引起了生物化工、医药工业研究领域的广泛关注。磁性壳聚糖微球具有表面非常光滑的球形结构。近年来,已经制备出了平均粒径在10～2.5×105 nm之间的磁性壳聚糖微球,并在生物医药、食品工程和污水处理等许多领域已经取得了初步的应用,特别是在污水处理和酶固定化领域。本文综述了近年来磁性氧化铁纳米粒子和磁性壳聚糖微球的制备方法、磁性壳聚糖微球的改性方法及应用的最新研究成果。     

Graft polymerization synthesis and application of magnetic Fe3O4/polyacrylic acid composite nanoparticles

Fe₃O₄ magnetic nanoparticles were prepared by coprecipitation using NH₃ · H₂O as the precipitating agent, and were characterized by Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), and X‐ray powder diffraction (XRD). The compatibility between the Fe₃O₄ nanoparticles and water were enhanced by grafting acrylic acid onto the nanoparticle surface. FTIR, XRD, thermogravimetry (TG), and differential scanning calorimetry (DSC) were used to characterize the resultant sample. The effects of initiator dosage, monomer concentration, and reaction temperature on the characteristics of surface‐modified Fe₃O₄ nanoparticles were investigated. Moreover, magnetic fluids (MF), prepared by dispersing the PAA grafted Fe₃O₄ nanoparticles in water, were characterized using UV–vis spectrophotometer, Gouy magnetic balance, and laser particle‐size analyzer. The rheological characteristics of magnetic fluid were investigated using capillary and rotating rheometers. The MF was added to prepare PVA thin film to improve mechanical properties. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007     

Preparation of inner asymmetric composite microspheres

Novel inner asymmetric composite microspheres were prepared by encapsulating surface‐modified magnetic particles via mini‐emulsion polymerization. Most of the surface‐modified magnetic particles encapsulated into the polymer matrix aggregate in one side of each microsphere, while only a few particles randomly disperse in the remaining part. The magnetic content of these novel asymmetric composite microspheres is 46.7% and the saturation magnetization is 23.8 emu g^?1. Copyright © 2012 Society of Chemical Industry     

Synthesis and characterization of air‐stable magnetic Fe composites microspheres of narrow size distribution

Air‐stable Fe magnetic nanoparticles entrapped within carbon and porous crosslinked polystyrene microspheres of narrow size distribution were prepared by the following sequential steps: (1) Polystyrene/poly(divinyl benzene) and polystyrene/poly(styrene‐divinyl benzene) uniform micrometer‐sized composite particles were prepared by a single‐step swelling of uniform polystyrene template microspheres dispersed in an aqueous continuous phase with emulsion droplets of dibutyl phthalate containing the monomers divinyl benzene and styrene and the initiator benzoyl peroxide. The monomers within the swollen polystyrene template microspheres were then polymerized by raising the temperature to 73°C; (2) Porous poly (divinyl benzene) and poly(styrene‐divinyl benzene) uniform crosslinked microspheres were prepared by dissolution of the polystyrene template part of the former composite particles; (3) Uniform magnetic poly(divinyl benzene)/Fe and poly(styrene‐divinyl benzene)/Fe composite microspheres were prepared by entrapping Fe(CO)₅ within the porous crosslinked microspheres, by suction of the Fe complex into the dried porous particles, followed by decomposition of the encapsulated Fe(CO)₅ at 200°C in Ar atmosphere; (4) Uniform magnetic air‐stable C/Fe composite microspheres were prepared similarly, apart from changing the decomposition temperature from 200 to 600°C. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

模板沉积法制备大孔高比表面积Fe3O4/P(GMA-co-EGDMA)磁性复合微球

介绍了一种以大孔高比表面积甲基丙烯酸缩水甘油酯（GMA）与二甲基丙烯酸乙二醇酯（EGDMA）共聚交联微球［P(GMA-co-EGDMA)］为模板制备磁性复合微球的简单方法。制备过程包括Fe³⁺和Fe²⁺的浸入、OH^-作用下孔内铁离子的共沉淀两步。在此过程中考察了浸泡温度、浸泡时间、共沉淀温度以及沉积次数对微球磁含量的影响,确定最佳制备工艺为50℃浸泡4 h,70℃反应1 h,如此反复4次磁含量可以达到45.24%。并通过SEM、VSM、XRD、TGA及压汞仪、激光粒度仪等手段对Fe₃O₄/P(GMA-co-EGDMA)的形貌、比饱和磁化强度、磁含量及孔性能进行了表征,微球的粒径范围处于100～200 μm之间,平均粒径为162 μm,比饱和磁化强度为10.92 emu·g^-1,平均孔径及比表面积分别为60 nm和116 m2·g^-1。     

Synthesis and characterization of novel conducting composites of Fe3O4 nanoparticles and sulfonated polyanilines

Surface charged iron oxide (Fe₃O₄) nanoparticles were used for the synthesis of sulfonated polyaniline (SPAN)‐Fe₃O₄ nanocomposites (SPAN/Fe₃O₄‐NCs). 2,5‐diaminobenzenesulfonic acid (DABSA) and 2‐aminobenzenesulfonic acid (ABSA) were independently polymerized with aniline to form SPAN. The structure of the composites was characterized by means of transmission electron microscopy (TEM), X‐ray diffraction (XRD), thermogravimetric analysis (TGA), Fourier transform infrared (FTIR) spectra, conductivity and magnetic properties. TEM reveals that Fe₃O₄ nanoparticles are “glued” with SPAN in the composite. TGA indicates that SPAN/Fe₃O₄‐NCs are having better thermal stability. The room temperature conductivity of SPAN/Fe₃O₄‐NCs is higher than that of pristine PANI and SPAN. SPAN/Fe₃O₄‐NCs exhibits magnetic behavior. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 104: 4127–4134, 2007     

柠檬酸钠改性的Fe3O4磁性纳米粒子的快速制备

以FeSO_4·7H_2O为单一铁源,浓氨水为沉淀剂,柠檬酸钠为表面改性剂利用简单回流法快速合成Fe_3O_4磁性纳米粒子。考察反应时间,反应温度及浓氨水加入方式对合成Fe_3O_4磁性纳米粒子的影响,并利用动态光散射仪、傅立叶红外射线光谱仪及透射扫描电镜等对合成的Fe_3O_4磁性纳米粒子进行表征。结果表明,以柠檬酸钠为表面改性剂,逐滴加入浓氨水,反应温度为(70～80)℃和反应时间为6 min时,获得的Fe_3O_4磁性纳米粒子在水中具有良好的分散性及磁响应性。Zeta电位和红外光谱同时表明,柠檬酸钠成功地吸附于Fe_3O_4磁性纳米粒子的表面(Fe_3O_4@SC),且Zeta电位值为-31.3 mV;透射扫描电镜显示获得的Fe_3O_4@SC磁性纳米粒子呈球状结构,粒径约为10 nm。     

表面双官能化的高分子复合磁性微粒的合成研究

以马来酸酐和2,6-二氨基吡啶反应得到的产物N-(6-氨基-2-吡啶基)马来酰胺酸作为功能基单体,与乙二醇二甲基丙烯酸酯(EGDMA)、聚乙二醇4000在引发剂偶氮二异丁腈(AIBN)存在下进行无皂乳液共聚合反应包裹磁性Fe3O4,制备了表面同时具有羧基和氨基的双官能化高分子复合磁性微球。采用扫描电镜、红外光谱等技术对所得材料进行了表征。考察了聚合温度、引发剂种类、反应时间、原料配比等参数对聚合物包裹磁性Fe3O4的影响。以AIBN为引发剂,Fe3O4、单体、交联剂比例为1︰1︰5,聚合反应时间6 h所得的复合磁性微粒具有较好的形貌、磁响应性能和94.3%的包裹率。