Nonionic latices in aqueous media part 1. Preparation and characterization of polystyrene latices

A series of non-ionic polystyrene latices in aqueous media containing particles with a narrow size distribution have been prepared using a nonyl phenol poly(ehylene glycol) condensate as the surfactant, methoxy poly(ethylene glycol methacrylate) as the comonomer/stabilizer, and ascorbic acid/hydrogen peroxide as the initiator system. As a control synthesis for comparison with the above latex, a charge stabilized polystyrene latex was prepared, using an anionic surfactant and potassium persulphate as the initiator. Latices employing a combination of charge plus steric stabilization mechanisms were also prepared, in order to investigate the effect of the non-ionic surfactant and the comonomer/stabilizer. The particle size of the latices was measured by transmission electron microscopy, the surface charge density by conductimetric titration and the glass transition temperature of the polymer by differential scanning calorimetry. The latex prepared using non-ionic ingredients, showed no titratable charge and exhibited a profound lowering of the glass transition temperature, with respect to the charge stabilized latex. On the basis of these results, schematic models for the polymerization mechanism and the morphology of the latex particles are proposed.     

Hematite nanoparticles as polystyrene microsphere coatings and hollow spheres: preparation and characterization

A novel method of fabricating composite particles with core–shell structures is demonstrated. The particles comprised monodisperse submicrometer-sized copolymer latex spheres as cores and Fe₂O₃ crystallites as shells. The shell was formed by controlled hydrolysis of aqueous iron solutions, and the growth of hematite on the surface of the copolymer spheres was controlled by slow injection. Hollow spheres were obtained by calcinations of the so-coated copolymer lattices at 500°C in air. The void size of these hollow spheres was determined by the diameter of the copolymer template, and the wall thickness could be easily controlled in the range of 20–60 nm by using this coating process. The structure and the composition of the spheres were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and thermogravimetric analysis (TGA). It can be seen that a crystallite change and a crystal phase transformation occurred during coating and calcination of the composite spheres. The formation of the composite particles is simply explained by the nucleation of iron oxide on the surface of the latex followed by growth of the iron compound shell.     

单分散超细二氧化钛颗粒的制备及粒径控制

四氯化钛和三乙醇胺在90 ℃反应生成钛可溶性化合物.该化合物溶液在145 ℃下陈化反应48 h,生成单分散性较好的锐钛矿型二氧化钛颗粒.讨论了钛可溶性化合物的形成和水解过程.陈化液的pH值在0.9～10.5变化时, 对颗粒大小和形状有显著的影响, 酸度越大, 颗粒越小.颗粒的大小也可以通过加入晶种得到控制.在pH为10.5时加入晶种, 颗粒的尺寸变小, 形貌基本维持棒状.用TEM和XRD等手段测定了颗粒的晶型、形貌和比表面积.     

氧缺位结构介孔二氧化钛/聚乙烯复合隔膜在锂硫电池中的应用

采用两步溶液法合成了一种具有高度氧缺位的黑色介孔二氧化钛, 并将其涂覆在隔膜表面作为锂硫电池复合隔膜, 研究了其在锂硫电池中的电化学性能. 结果表明, 氧缺位的黑色介孔二氧化钛材料不仅展现出良好的导电性, 还能加强对多硫化物的物理和化学吸附能力, 从而显著提高锂硫电池的放电比容量(0.1C倍率下首次放电比容量为1257 mA·h/g)和循环性能(循环100次后放电比容量为821 mA·h/g).     

Preparation and characterization of polysiloxane-poly(butyl acrylate-styrene) composite latices and their film properties

Gamma ray induced seeded emulsion co-polymerization of styrene and butyl acrylate was carried out in the presence of polymerizable polysiloxane seed latex which was obtained by the ring opening co-polymerization of octamethyl cyclotetrasiloxane (D₄) and tetramethyl tetravinyl cyclotetrasiloxane (VD₄) catalyzed by dodecylbenzene sulphonic acid (DBSA). A series of polysiloxane seed latices with different molecular weight, vinyl content, and particle size were used. The conversion-time curve showed that the polymerization rate was accelerated much by the seed latex. The obtained composite latices also showed good storage stability, mechanical stability and high electrolyte resistance ability. The morphology of the composite latex particles was found to be a quite uniform fine structure by transmission electron microscope (TEM). The graft polymerization between polymerizable polysiloxane and butyl acrylate or styrene was confirmed by the Fourier transform infrared spectroscopy (FT-IR) and the graft efficiency was also studied. The influence of seed content, molecular weight, vinyl content of the polysiloxane and seed latex particles size to the mechanical performance, water absorption ratio, surface properties, transparency and UV resistance of the latex films, was also investigated.     

Facile fabrication of hollow silica and titania microspheres using plasma-treated polystyrene spheres as sacrificial templates

By means of a plasma technique, the surfaces of monodisperse polystyrene (PS) colloids have been modified with hydroxyl groups. Using these surface-modified PS colloids as sacrificial templates, we have fabricated silica-coated PS colloids (PS@silica) and titania-coated PS colloids (PS@titania) composite microspheres as well as hollow and mesoporous silica and titania microspheres. This process not only demonstrated a facile, low-cost, environmentally benign way to fabricate hollow oxides structures but also offered a feasible alternative to the preparation of polymer/inorganic oxide composites by templating against the polymer substrate with hydrophobic surfaces.     

Titanium dioxide nanowires as green and heterogeneous catalysts for the synthesis of novel pyranocoumarins

Titanium dioxide nanowires were employed as novel, recyclable and safe catalysts in a one-pot three-component condensation of aldehydes, malononitrile, and 4-hydroxycoumarin to produce new and known pyrano[2,3-c]chromenes as potent biologically active compounds. A possible catalytic mechanism was also proposed based on the interaction of reactants with TiO₂ nanowires. This expedient new route has advantages, such as the use of a safe and reusable catalyst, simple operation, short reaction times and good to excellent yields.     

Synthesis and Characterization of Mesoporous Titanium Dioxide Spheres

Mesoporous titanium dioxide spheres were synthesized by a convenient solvothermal method at room temperature with tetraethyl titanate as a precursor. Investigation by means of X-ray diffraction(XRD), transmission electron microscopy(TEM), scanning electron microscopy(SEM), and N2 adsorption-desorption isotherms confirms that the sample has a mesostructure with a higher specific surface area and shows that the mesoporous TiO2 spheres have a diameter of 2 μm, the average pore size is about 5.9 nm, and the BET...     

离子掺杂改性纳米TiO_2光催化剂的研究进展

以纳米TiO2为代表的纳米半导体光催化材料是目前研究的热点。纳米TiO2为宽禁带半导体,需紫外光激发;而且,产生的光生电子-空穴对极易复合,限制了其实际应用。将纳米TiO2进行离子掺杂改性是解决上述问题的有效途径。目前离子掺杂改性纳米TiO2光催化剂的研究进展表明,采用两种离子共掺杂改性纳米TiO2时,离子之间会产生协...     

Titanium Dioxide as a Mild and Efficient Catalyst for Conversion of Epoxides to Thiiranes

Abstract

Titanium dioxide (TiO₂) efficiently catalyze the reaction of a variety of epoxides with ammonium thiocyanate in refluxing acetonitrile to afford the corresponding thiirane in high to excellent yields.     

Influence of Titanium Dioxide Content on the Crystallization Behavior and Solar Reflectance of Polyethylene/Titanium Dioxide Composites

Titanium dioxide (TiO₂) particles were introduced to improve the solar reflectance of high-density polyethylene (HDPE). The organic-inorganic hybrids were fabricated by melt blending. A series of characterizations were taken to study the crystallization behavior, morphology, solar reflectance, and real cooling property. TiO₂ particles acted as nucleation agents in the HDPE matrix and made the HDPE form thick lamellar crystals. TiO₂ particles could disperse well into the HDPE matrix under 2.5 wt.% loading but agglomerated with 3 wt.%. Solar reflectance was related to the reflective index of TiO₂ and the microstructure of HDPE. The real cooling property depended on the solar reflectance and the dispersion of the TiO₂ particles in the HDPE matrix.     

电化学溶解钛金属直接水解法制备纳米TiO_2

纳米材料是目前材料科学的热点 .TiO2作为一种重要的无机功能材料 ,具有温敏、气敏、光催化等功能 ,广泛用于光电材料、涂料、传感器、介电材料、催化剂及载体等重要领域 .由于其各种应用都与粉体的性能有直接关系 ,因此研究纳米 TiO2的制备方法具有重要的实际意义 [1].近年来 ,纳米 TiO2粉体制备方法有了很大的发展 ,如 TiCl4气相水解沉淀法 [2],乳浊液法和 Ti(OC4H9)4水解沉淀法 [1],喷雾热解法 [3],放电爆炸法 [4],反应电极埋弧法 [5],溶胶凝胶 (Sol gel)法 [6]等 ,其中溶胶凝胶法是制备纳米材料的有效方法 .但这些方法存在…     

Synthesis of polystyrene/SiO2 composite microparticles by dispersion polymerization in supercritical fluid

A novel synthetic route to prepare polystyrene/SiO₂ composite microparticles in supercritical carbon dioxide (scCO₂) is presented. Silica particles with the size of 130 nm which were surface-modified with 3-(trimethoxysilyl) propyl methacrylate were used as seeds in the dispersion polymerization of styrene in the presence of a polymeric stabilizer, poly(1,1-dihydroheptafluorobutyl methacrylate-co-diisopropylaminoethyl methacrylate) to produce dry composite particles. The transmission electron microscopy analysis revealed that the composite microspheres contained several silica particles.     

Synthesis and properties of silica/polystyrene/polyaniline conductive composite particles

In this study, silica/polystyrene/polyaniline (SiO₂/PS/PANI) conductive composite particles were synthesized by four sequential reactions. The nanosized SiO₂ particles were synthesized from tetraethoxysilane (TEOS) by a sol–gel process with water as the solvent medium, followed by a surface modification with triethoxyvinylsilane; then the surface modified SiO₂ particles were used as seeds to synthesize SiO₂/PS composite particles with soapless seeded emulsion polymerization. Finally, the SiO₂/PS particles were used as seeds to synthesize the SiO₂/PS/PANI conductive composite particles. The sol–gel process of SiO₂, the effect of surface modification, and several other factors that influenced polymerization of styrene in the soapless seeded emulsion polymerization will be discussed. Either potassium persulfate (KPS) or 2,2′‐azobis(isobutyramidine) dihydrochloride (AIBA) was used as the initiator to synthesize the uniform SiO₂/PS particles successfully, and the cross‐section morphology of the SiO₂/PS particles was found to be of a core–shell structure, with SiO₂ as the core, and PS as the shell. The SiO₂/PS particles were well dispersed in many organic solvents. In the following step to synthesize SiO₂/PS/PANI conductive composite particles, sodium dodecyl sulfate (SDS) played an important role, specifically, to absorb aniline onto the surfaces of the SiO₂/PS particles to carry out the polymerization of aniline over the entire surface of the particles. The conductivity of the SiO₂/PS/PANI composite particles approached that of semiconductive materials. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 43: 342–354, 2005     

Synthesis and characterization of sulphonated core-shell latices in the size range between 30 and 80 nm

The objective of the current work was the synthesis of sulphonated core-shell nanolatices and to investigate to which extend it is possible to control the final surface charge of such latices. For this purpose differently sized polystyrene seed latices with average diameters in the size range between 30 and 80 nm were synthesized by emulsion polymerization. To obtain the final latices, a sulphonated comonomer was incorporated in the outer surface shell of the particles by further reaction of the seed latices with styrene and sodium styrene sulphonate (NaSS). In a first test series the seed latex surface was modified with four different amounts of NaSS. In a second test series four different seed latices were reacted with the same amount of NaSS. In the last set of reactions the seed latices were reacted with different amounts of NaSS and in these reactions the ratio of added NaSS to the specific surface area of the seed latex was kept constant to obtain differently sized latices of the same surface charge density. The yield of sulphonic acid groups in the particle shell was found between 57 and 74% after an intensive cleaning step by ion exchange. The results show possibilities for a reproducible synthesis of small sulphonated latex particles with a desired surface charge density.     

磁性二氧化钛纳米粒子的制备及其光催化性能

以硫酸钛和Fe3O4为原料, 采用共沉淀法制备了掺杂不同量Fe3O4的磁性纳米TiO2 (Fey-TiO2+x) , 通过X-射线衍射(XRD)、热重-差示扫描量热(TG-DSC)、紫外-可见吸收光谱(UV-Vis) 和荧光光谱等分析手段对样品的晶体类型、光谱吸收特征和磁响应性等进行了表征;以太阳光为光源, 考察其对甲基橙的光催化降解活性. 结果表明, Fey-TiO2+x纳米粒子主要以锐钛矿相存在, 粒子的粒径约为12 nm;在8 mT外加磁场作用下, 粒子悬浮液的吸光度在12 min内减少70%, 而无外加磁场时仅减少25%, 说明Fey-TiO2+x纳米粒子具有良好的磁响应性. Fe2+和Fe3 +离子掺入TiO2 后, 使TiO2晶格形成缺陷, 使吸收带边由380 nm 红移到460 nm, 从而提高了TiO2对可见光的吸收效率. Fe的最佳掺杂量为Ti的0.05%(摩尔比), 该催化剂在240 min内对甲基橙的降解率接近100%;加入少量H2O2能显著提高Fe0.05-TiO2的光催化性能, 在20 min内对甲基橙的降解率即接近100%.     

TiO2颗粒表面包覆SiO2纳米膜的动力学模型

针对液相法二氧化钛颗粒表面包覆氧化硅纳米膜的过程,提出包覆过程是溶胶凝胶机制,研究了表面成膜的动力学方程,考察了成膜剂浓度和成膜过程中温度对成膜速度的影响,并通过实验对氧化硅膜形成的动力学方程进行了验证.     

包覆型磁性二氧化钛的制备及其光催化性能的研究

采用表面改性的方法分别制备了两种核-壳和核-壳-壳式结构的TiO2/γ-Fe2O3,TiO2/S iO2/γ-Fe2O3包覆型磁性二氧化钛.用XRD、TG-DTA、TEM、BET、和IR等手段对样品进行了结构表征,并研究了它们在紫外光照射下对甲基橙的降解性能.结果表明,在紫外光的照射下,包覆型磁性二氧化钛可有效地降解甲基橙;TiO2/S iO2/γ-Fe2O3的光催化活性优于TiO2/γ-Fe2O3,前者在循环使用三次后降解率仍不低于95%.     

Composites Based on Polystyrene Microspheres with Nano-Scaled Titanium Dioxide

This study produced for the first time composites based on polystyrene microspheres with nano-sized titania synthesized by sulfate and sol-gel methods, as well as commercial Hombifine N, Hombikat UV100, and Degussa P25. The starting samples and the composites were characterized by X-ray diffraction, scanning electron microscopy, nitrogen adsorption capacity, and IR spectroscopy. The highest content of nano-titanium dioxide both in the bulk and on the surface of microspheres was obtained with the use of Hombikat UV100. This sample has the largest specific surface area and a high content of reactive OH groups. The adsorption properties of composites were investigated.     

Characterization of Titanium Dioxide Nanoparticles on Porcine Skin by Raman Microscopy

Titanium dioxide nanoparticles are a key ingredient in sunscreen products for efficiently blocking ultraviolet irradiation on the skin. Lately, there have been concerns about their cytotoxicity, oxidative stress, and DNA damage to skin cells. One way to minimize the potential side effects is to wash away the nanoparticles from skin. However, the effectiveness of this strategy has not been evaluated, which is partially due to the lack of a convenient technology for skin analysis. Herein, a portable Raman microscope was shown for the first time to rapidly reveal and quantify titanium dioxide nanoparticle residue on the skin after cleaning. By using porcine skin as an example, cleaning with the detergent was determined as the fastest and most efficient way to remove the nanoparticles from the skin.