Silica sol/Nano-Au/PVP修饰金电极电致化学发光测定槐定碱

基于槐定碱对联吡啶钌（Ru（bpy）3^2＋）在电致化学发光中的增敏机理,通过传感器修饰技术,将Silica sol/Nano-Au/PVP修饰到金电极表面,建立了简单、快捷测定槐定碱的新方法。实验表明,最佳实验条件下,在1.6×10^-7-1.6×10^-4mol/L范围内,槐定碱的浓度与其对应的电化学发光强度值呈良好的线性关系,I=4.000×10^7c＋262.2,r^2=0.994 5,检出限（S/N=3）为3.5×10^-9mol/L。连续平行测定浓度为1.6×10^-5mol/L的槐定碱溶液6次,其相对标准偏差（RSD）为2.9%。该方法具有较高的选择性和灵敏度,样品处理简单快速,用于槐定碱的测定,结果满意。

溶胶-凝胶法改良人工林马尾松尺寸稳定性及其机理研究

马尾松是广西地区重要的人工林资源之一,但其尺寸稳定性较差,极大地限制了其在木材工业中的使用。本研究选用基于SiO_(2)的溶胶-凝胶法对马尾松进行改良,探讨了浸渍时间对马尾松尺寸稳定性的影响,并通过扫描电子显微镜(SEM)、X射线能谱(EDS)、傅里叶变换红外光谱(FT-IR)、X射线光电子能谱(XPS)、X射线衍射(XRD)揭示了溶胶-凝胶法对马尾松的改良机理。研究结果表明:经过6 h溶胶浸渍处理的改性马尾松尺寸稳定性最好,相较于未处理的马尾松,浸渍6 h的改性马尾松的浸渍率为5%,60 h吸水质量增加率由34.7%降低至28.2%,60 h吸湿体积膨胀率由16.5%降低至11.1%,72 h抗老化性能由18.02的色差值降低为11.9。溶胶-凝胶法对马尾松尺寸稳定性的改善机理体现在两个方面:其一,通过形成玻璃层状及膨胀结构可以阻挡水分的进入;其二,通过氢键及化学键的形式与细胞壁进行结合,以起到永久的润胀作用。

Nano-Au/Silica sol/PVP修饰金电极上电化学发光测定盐酸硫必利

采用溶胶-凝胶法制备了Nano—Au／Silicasol／PVP修饰金电极，并基于盐酸硫必利对联吡啶钌（Ru（bpy）2/3＋）在该修饰电极上弱电化学发光具有较强的增敏作用，建立了电化学发光检测盐酸硫必利的新方法。在最佳实验条件下，盐酸硫必利浓度在1．0×10-7～1．0×0-4mol／L范围内与相对发光强度呈线性关系（r2=0．9978），检出限（S／N-3）为6．7×10-10mol／L。连续平行测定1．0×10-5mol／L盐酸硫必利溶液10次，发光强度的相对标准偏差（RSD）为1．789／6。对样品进行回收率试验，其回收率在97．7％～103．9％之间，RSD为2．62％。该方法具有较高的选择性和灵敏度，样品处理简单快速，用于盐酸硫必利的测定，结果满意。

硅溶胶-异丁基三乙氧基硅烷复合乳液对泡沫混凝土防水性能的影响

[目的]研究硅溶胶-异丁基三乙氧基硅烷(IBTS)复合乳液对泡沫混凝土防水性能的影响,为拓宽其应用提供实验数据。[方法]通过宏观力学特性试验和微观结构分析,综合考察了该复合乳液对泡沫混凝土的防护效果。[结果]涂抹了复合乳液的泡沫混凝土表现出比涂抹了单一IBTS乳液的泡沫混凝土更优异的抗渗透性能和耐久性,其水渗透深度和碳化深度更小,浸水48 h后的吸水率为0.46%,氯离子迁移系数为1.1×10^(-12)m^(2)/s,冻融240次后的质量损失率为0.55%,且动弹性模量仍维持冻融试验前的85.34%。[结论]复合乳液的防水机理涉及表面效应、化学反应、物理效应等多个方面,通过形成致密的防水层、填充孔隙和微裂纹、吸附并包固水分子等方式来防止水分渗透和扩散,从而提高泡沫混凝土的防水性能。

隔热填料对硅溶胶-苯丙乳液复合涂料光反射和隔热性能的影响

为了降低太阳光辐射给建筑物带来的能源损耗,提高涂料的隔热效果,主要研究了钛白粉、氧化铝、滑石粉、SiO_(2)气凝胶的含量对硅溶胶-苯丙乳液复合涂料性能的影响。通过对比实验制备了涂料样品,并测试了涂料的性能,确定各填料的最佳含量。结果表明:钛白粉和氧化铝的最佳含量分别为12%和2%,此时涂料具有较好的反射率。滑石粉含量在8%时涂料具有较高的硬度。SiO_(2)气凝胶含量在4%时涂料的隔热效果最好,隔热温差为8℃。通过微观形貌表征发现,SiO_(2)气凝胶含量超过4%之后涂料开始出现裂纹。选择各填料的最佳用量,制备了硅溶胶-苯丙乳液复合型隔热涂料,根据建筑涂料体系产品技术要求的标准测试了涂料的耐水性、耐碱性等性能,测试结果均合格。

Preparation and Characterization of Hybrid Aqueous Dispersions Composed of Silica Sol and Poly(styrene-co-acrylate)

A stable silica sol with 3-5 nm in diameter, which can form homogeneous film without crack, was prepared and characterized. Then, the inorganic-organic hybrid aqueous dispersion composed of such a silica sol and an emulsion of styrene （St） and acrylate （Ac） copolymer was prepared and the hybrid effect between the silica sol and poly（St-co-Ac） was observed by Fourier transform infra-red （FT-IR） spectroscope. The toughness of the film prepared by this kind of hybrid aqueous dispersion was excellent, as it was enhanced appreciably by commixing with a small amount of poly（St-co-Ac） emulsion. Some amino-polysiloxane modified hybrid aqueous dispersions were also prepared and the properties of the modified dispersions and their films were investigated. The experimental results showed that the film prepared with such an amino-polysiloxane modified hybrid dispersion exhibited excellent hydrophobicity and low surface energy after heat treatment for 1.5 h, during which the formation of the graft copolymer was observed. The surface energy of this film decreases as a result of the enrichment of siloxane segments on the film surface.

SYNTHESIS OF MESOPOROUS POLY(STYRENE-co-MALEIC ANHYDRIDE)/SILICA HYBRID MATERIALS VIA A NONSURFACTANT-TEMPLATED SOL-GEL PROCESS

Mesoporous poly(styrene-co-maleic anhydride)/silica hybrid materials have been prepared. The synthesis was achieved by the HCl-catalyzed sol-gel reactions of tetraethyl orthosilicate (TEOS) and styrene-maleic anhydride copolymer in the presence of 3-aminopropyl triethoxysilane (APTES) as a coupling agent and citric acid as a nonsurfactant template or pore-forming agent, followed by ethanol extraction. Characterization results from nitrogen sorption isotherms and powder X-ray diffraction indicate that polymer-modified mesoporous materials with large specific surface areas (e.g. 900 m(2)/g) and pore volumes (e.g. 0.6 cm(3)/g) could be prepared. As the citric acid concentration is increased, the specific surface areas, pore volumes and pore diameters of the hybrid materials increase.

Microstructure Control of Nanoporous Silica Thin Film Prepared by Sol-gel Process

Nanoporous silica films were prepared by sol-gel process with base, acid and base/acid two-step catalysis.Transmission electron microscope （TEM） and particle size analyzer were used to characterize the microstructure and the particle size distribution of the sols. Scanning electron microscopy （SEM）, atomic force microscopy （AFM） and spectroscopic ellipsometer were used to characterize the surface microstructure and the optical properties of the silica films. Stability of the sols during long-term storage was investigated. Moreover,the dispersion relation of the optical constants of the silica films, and the control of the microstructure and properties of the films by changing the catalysis conditions during sol-gel process were also discussed.

Preparation and characterization of silica microcapsules containing butyl-stearate via sol-gel method

For thermal energy storage application in energy-saving building materials,silica microcapsules containing phase change material were prepared using sol-gel method in O/W emulsion system. In the system droplets in microns are formed by emulsifying an organic phase consisting of butyl-stearate as core material. The silica shell was formed via hydrolysis and condensation from tetraethyl silicate with acetate as catalyst. The SEM photographs show the particles possess spherical morphology and core-shell structure. The as-prepared silica microcapsules mainly consist of microsphere in the diameter of 3-7 μm and the median diameter of these microcapsules equals to 5.2 μm. The differential scanning calorimetry(DSC) curves indicate that the latent heat and the melting point of microcapsules are 86 J/g and 22.6 ℃,respectively. The results of DSC and TG further testify the microcapsules with core-shell structure.

Preparation of Scratch-Resistant Nano-Porous Silica Films Derived by Sol-Gel Process and Their Anti-reflective Properties

Structural strengthening of the nano porous silica films has been reported. The films were prepared with a base/acid two-step catalyzed TEOS-based sol-gel processing and dip-coating, and then baked in the mixed gas of ammonia and water vapor. The silica films were characterized with TEM, AFM, FTIR, spectrophotometer, ellipsometer, and abrasion test, respectively. The experimental results have shown that the films have a nanostructure with a low refractive index and can form an excellent scratch-resistant broadband anti-reflectance. The two-step catalysis noticeably strengthens the films, and the mixed gas treatment further improves mechanical strength of the silica network. Finally the strengthening mechanism has been discussed.

Experiment on the silica sol imbibition of low-permeability rock mass:With silica sol particle sizes and rock permeability considered

It’s a universal engineering problem to seal micro-cracks of low-permeability argillaceous rock mass by grouting in the fields of civil engineering and mining.This paper achieved the grouting sealing of lowpermeability artificial rocks with the permeability of 0.1–40 mD by adopting silica sol imbibition grouting.The variation characteristics of particle size,viscosity,and contact angle of silica sol during solidification and the pore size distribution of low-permeability artificial rocks were measured,and spontaneous imbibition tests of the artificial rocks were carried out.Finally,combined with the imbibition theory,percolation theory,and fracture medium grouting principle,the silica sol imbibition mechanism of lowpermeability rocks and soil was discussed.The results show that:(1)Silica sol can be injected into artificial rocks with the minimum permeability of 0.1 mD through spontaneous imbibition;(2)The particle size increase of silica sol leads to decreased wettability,affinity,and injectability in grouting materials;and(3)In the range of 0.1–40 mD,the grout absorption first increases and then decreases with increased permeability.The number of large pores and fractures in the rock mass is related to injectability,and the number of small and medium pores is related to the internal driving force of imbibition.This study provides a theoretical basis for silica sol grouting sealing of low-permeability argillaceous rocks and is,therefore,an important reference for application.

Effects of Silica Sol on Structure and Properties of Core-Shell Silicon-Acrylic Materials

Silica sol prepared by sol-gel method was introduced into poly (butyl acrylate) (PBA)/poly (butyl acrylate-styrene-methacryloxypropyl trimethoxysilane) (PSBM) core-shell emulsions to prepare a series of paper surface sizing agents. The rheological measurement indicated that PSBM emulsions exhibited shear-thinning behavior, and the phenomena became more pronounced with increasing silica sol concentration. Dynamic mechanical analysis (DMA) demonstrated that the stronger interfacial interaction between silica sol and polymer matrix, but microphase separation took place with excess silica sol. Thereby the tensile strength and thermal stability of emulsion films were increased with desirable silica sol concentration, and when silica sol concentration was greater than 6 wt%, the tensile strength leveled off and the decomposition temperature decreased from 351.19℃ to 331.63℃. The degree of crystallinity increased from 5.12% to 10.98% with 4% silica sol addition, resulting in enhanced rigidity of films. Furthermore, the interaction between polymer and fiber was improved with certain amount of silica sol, resulting in improved sizing degree, ring crush strength, surface strength and folding strength. However, excessive crosslinking will be harmful for the properties of sized paper.

硅溶胶-酚醛树脂共结合Al_(2)O_(3)-SiC-C砖性能研究

为了缓解酚醛树脂碳化引起的Al_(2)O_(3)-SiC-C砖组织结构劣化,提升Al_(2)O_(3)-SiC-C砖的力学性能和抗渣性能,以粒度分别为5~3、3~1和≤1 mm的高铝矾土为骨料,以电熔白刚玉(≤0.045 mm)、SiC(≤0.075 mm)、α-Al_(2)O_(3)微粉和鳞片石墨(≤0.15 mm)等为基质,以热固性酚醛树脂和硅溶胶为结合剂,制备了硅溶胶-酚醛树脂共结合Al_(2)O_(3)-SiC-C砖。在酚醛树脂外加量为4.5%(w)的基础上,探究了硅溶胶的加入量(外加质量分数分别为0、0.45%、0.90%和1.35%)对Al_(2)O_(3)-SiC-C砖常温力学性能、高温力学性能和抗渣性能的影响。结果表明:引入适量硅溶胶可以有效提升Al_(2)O_(3)-SiC-C砖的力学性能及抗渣性能,当硅溶胶加入量为0.45%(w)时,试样具有优异的常温、高温力学性能及抗渣性能。

STUDIES ON SYNTHESIS OF SILICA SOL-ORGANIC POLYMER COMPOSITE EMULSION

An emulsion of polystyrene/poly (butylacrylate-methyl methacrylate acrylic acid) core/shell latex particles (PS/P (BA-MMA-AA)) has been prepared by use of three synthetic methods. The effects of synthetic methods on the distribution of carboxyl groups in latex particles were studied. The results show that the seed emulsion polymerization in which the pre-emulsified monomers were added by dropping method to the second stage is the best technique for obtaining the optimum distribution of carboxyl groups on the surface of the latex particles. Furthermore, by using PS/P (BA-MMA-AA), a type of novel composite emulsion of silica sol-PS/P (BA-MMA-AA) was synthesized with the above method. By observation through transmission EM, the morphology of the latex particles obtained shows that a composite structure has been formed between silica sol particles and organic polymer particles.

Facile and Controlled Synthesis of Silica Sol Nanospheres Through a Modifi ed Sol-Gel Process

An effective and reproducible preparation of silica sol nanospheres via a modified sol-gel process has been described. Monodisperse and stable silica sol nanospheres with uniformsize were successfully obtained through the optimized synthesis in which the mixture of tetraethyl orthosilicate （TEOS） and ethanol was followed by the addition of water and ammonium hydroxide （NH3） separately, and the size of silica sol spheres was strictly controlled in the range of 25-119 nm with a narrow size distribution by fine adjustment of several reaction parameters. Results showed that in the presence of low concentration of TEOS, spheres size rose first and reached maximum when H2O concentration was up to 66 g/L. However, the diameter of silica sol spheres decreased above 66 g/L of H2O concentration. Furthermore, it was also found that the size and size distribution of silica sol nanospheres were affected by NH3 concentration. As NH3 concentration increased from 15 to 35 g/L, the diameter declined from 83 to 64 nm. Nevertheless, higher NH3 concentration would result in relatively broad size distribution, and gelation occurred when NH3 concentration reached 44 g/L. In addition, the effect of the different feed rates ofNH3 on the size growth of silica sol nanospheres was also discussed.

Immobilization of Functionalized Ionic Liquid on Sol-Gel Derived Silica for Efficient Removal of H_2S

An innovative approach to H2 S capture has been developed using several metal-based ionic liquids([Bmim]Cl·CuCl_2, [Bmim]Cl·FeCl_3, [Bmim]Cl·ZnCl_2, [Bmim]Br·CuCl_2, and [Bmim]Br·FeCl_3) immobilized on the sol-gel derived silica, which is superior to purely viscous ionic liquid with a crucial limit of high temperature, low mass transfer rate,and mass loss. The adsorbents were characterized by the Fourier transform infrared spectrometer, transmission electron microscope, N_2 adsorption/desorption, X-ray photoelectron spectroscopy, and thermal analysis techniques. The effects of the metal and halogen in IL, the loading amount of IL, and the adsorption temperature were studied by dynamic adsorption experiments at a gas flow rate of 100 mL/min. The H2 S adsorption results have showed that the optimal adsorbent and adsorption temperature are 5% [Bmim]Cl·CuCl_2/silica gel and 20—50 ℃, respectively. H_2 S can be captured and oxidized to elemental sulfur, and [Bmim]Cl·CuCl_2/silica gel can be readily regenerated by air. The excellent efficiency of H2 S removal may be attributed to the formation of nano-scaled and high-concentration [Bmim]Cl·CuCl_2 confined in silica gel, indicating that the immobilization of [Bmim]Cl·CuCl_2 on the sol-gel derived silica can be used for H2 S removal promisingly.

Effect of Catalyst on the Formation of Silica Coating on Nickel Substrate by Sol-Gel Processing

In this research work silica coating was produced on nickel substrates by a sol-gel process. In order to increase the rate of hydrolysis and to reduce the rate of polymerization several acid catalysts including nitric acid-hydrochloric acid, acetic acid, hydrochloric acid and nitric acid were add to silica sol. Conversely, in order to control the rate of hydrolysis and to increase the rate of polymerization, basic catalyst of ammonia and ammonia hydroxyl were introduced in to the solution. Nickel specimens of known surface roughness were chemically cleaned and prepared by dipping in the sols. In order to produce a suitable silica coating the drying and firing cycles were optimized on these substrates. The structure and uniformity of the coatings produced were examined by scanning electron microscopy. Coatings composition was determined using glow discharge optical spectroscopy and EDAX microanalysis. Experimental result showed that hydrochloric acid, acetic acid, ammonia and acetic acid - ammonia are suitable catalytic agents for silica coating formation on nickel type substrate.

Formation of macroporous gel morphology by phase separation in the silica sol-gel system containing nonionic surfactant

The phase separation and gel formation behavior in an alkoxy-derived silica sol-gel system containing C16EO15 has been investigated. Various gel morphologies similar to other sol-gel systems containing organic additives were obtained by changing the preparation conditions. Micrometer-range interconnected porous gels were obtained by freezing transitional structures of phase separation in the sol-gel process. The dependence of the resulting gel morphology on several important reaction parameters such as the starting composition, reaction temperature and acid catalyst concentration was studied in detail. The experimental results indicate that the gel morphology is mainly determined by the time relation between the onset of phase separation and gel formation.

RHEOLOGICAL MODIFICATION OF EPOXY RESINS WITH NANO SILICA PREPARED BY THE SOL-GEL PROCESS

Nano silica-modified epoxy resins were synthesized by the sol-gel process, The materials have the morphological structure of nano particales dispersed in the epoxy matrix. The dispersed phase formed a physical network in the resin and thus influenced the rheological behavior greatly. However, the nano silica did not show a significant influence on the mechanical properties of the cured resins.

Preparation and Characterization of Silica and Clay-Silica Core-Shell Nanoparticles Using Sol-Gel Method

Silica and montmorillonite-supported silica nanoparticles were prepared via an acid one step sol-gel process. The synthesized solids were characterized using XRD, FTIR, TEM and N2 adsorption. The effect of preparing temperatures on the structure and properties of the silica nanoparticles were studied. The results show that the increase of annealing temperature from 25 to 200℃, don’t change amorphous state of silica. While for montmorillonite-supported silica the clay platelets are delaminated during the sol-gel process. TEM results showed that the average particle size of silica is increased by increasing temperature due to the particle sintering and the clay-silica nanoparticles possessed core–shell morphology with diameter of 29 nm. The surface area measurements showed that by increasing annealing temperature the surface area was decreased due to aggregation of particle. The clay-silica sample showed lower average pore width than that of the silica prepared at 200℃ indicating that it has a macropores structure. The adsorption efficiency of the prepared samples was tested by adsorption of protoporphyrin IX. The highest adsorption efficiency was found for SiO2 prepared at 200℃. Temkin model describe the equilibrium of adsorption of protoporphyrin IX on caly-silica nanoparticles under different conditions.