Synthesis of ultrafine silica powders based on oil shale ash by fluidized bed drying of wet-gel slurry

Ultrafine silica powders were synthesized using oil shale ash which is a solid by-product of oil shale processing. Fluidization technique was employed for the drying of wet-gel slurry at an ambient pressure. Box-Behnken statistical design was used to optimize the factors affecting the extraction efficiency of the silica such as concentration of sodium hydroxide, reaction time and reaction temperature, and to determine the optimum conditions for the extraction process. The result of statistical design shows that the extraction efficiency was in an agreement with the generated model and the experimental results. It is observed that the extraction efficiency of silica was increased by increasing the concentration of sodium hydroxide, the reaction time and the reaction temperature. Further, the ultrafine silica powders were characterized by transmission electron microscopy (TEM), X-ray fluorescence spectroscopy (XRF) and nitrogen adsorption (using BET equation). The BET surface area of the ultrafine silica powders obtained in fluidized bed is comparatively higher (652 m²/g) than that of silica powders dried in the furnace (385 m²/g). It is clear that the properties of silica powders obtained in fluidized bed are superior to that of powders dried in the furnace.     

纳米润滑油添加剂技术的研究进展

物理、化学性质特殊的纳米粒子在摩擦学领域引起了人们极大的兴趣,本文主要从纳米润滑油添加剂的结构与特性,摩擦学性能与润滑机理,纳米材料作为润滑油添加剂存在的问题及解决方法等几方面,介绍了纳米润滑油添加剂技术的研究进展,展望了纳米润滑油添加剂的发展前景,并指出了需要进一步深入研究的几个问题。     

响应面法优化中空介孔二氧化硅球包载吲哚美辛的工艺研究

采用硬模板法在室温下、中性水溶液中合成了中空介孔二氧化硅球,中空部分直径为250nm,外壳厚度25nm。利用氮气吸附-解吸附、透射电子显微镜、傅里叶变换红外光谱表征了微球的物理化学性质。该微球球形度良好,BET结果显示其比表面积为730.0m²/g,平均孔容1.084cm³/g ,平均孔道直径6.58nm。利用中空介孔二氧化硅球较好的载药性能负载吲哚美辛,并采用三因素的Box-Behnke实验设计对药物负载处方工艺进行优化研究。当IMC/HMSNs质量比为22:1,超声1.4h,震荡吸附23h时实验条件达到最佳,包封率理论值为85.2%。在此条件进行验证实验,吲哚美辛的包封率可达理论预测值的98.7%,说明将 Box-Behnken 实验设计法用于中空介孔二氧化硅球包载吲哚美辛的优化筛选是可行的,且得到的实验观察值与数学模型的预测值相符合。     

Modelling of relation between synthesis parameters and average crystallite size of Yb2O3 nanoparticles using Box-Behnken design

A straightforward wet chemical method has been applied for the fabrication of Yb₂O₃ nanoparticles (NPs) from ytterbium nitrate solution by using ammonium carbonate as precipitation agent. Effects of precursor molarity (0.1, 0.15 and 0.2 M), calcination temperature (800, 900 and 1000 °C) and time (2, 4 and 6 h) on average crystallite size (CS) of the NPs were statistically investigated by using Box-Behnken design. A simple and effective quadratic model was proposed for controlling the CS. The CS values were calculated by using Williamson Hall method (W-H) from X-Ray Diffraction (XRD) broadening data and found to be ranging between 13 and 26 nm. Agglomerated NPs morphologies and particle sizes were revealed by Field Emission Gun-Scanning Electron Microscopy (FEG-SEM). Fourier Transform Infrared (FTIR) spectrophotometry confirmed that as-received Yb₂(CO₃)₃xH₂O powders were successfully transformed into Yb₂O₃ NPs with calcination. High-Resolution Transmission Electron Microscopy (HRTEM) results verified the average CS values. ANOVA analyses revealed that linear and squared terms of the production parameters were significantly related to the CS whereas interaction terms were insignificant with the confidence level of 95% (R² = 92.67%, R²-adj = 87.17%). The calcination temperature had the highest impact on the average CS followed by the time and precursor molarity. Increasing calcination parameters resulted in bigger crystallites whereas increasing precursor molarity exhibited a critical supersaturation value (0.15 M) from which the average CS was decreased.     

Preparation and optimization of matrix metalloproteinase-1-loaded poly(lactide-co-glycolide-co-caprolactone) nanoparticles with rotatable central composite design and response surface methodology

Matrix metalloproteases are key regulatory molecules in the breakdown of extracellular matrix and in inflammatory processes. Matrix metalloproteinase-1 (MMP-1) can significantly enhance muscle regeneration by promoting the formation of myofibers and degenerating the fibrous tissue. Herein, we prepared novel MMP-1-loaded poly(lactide-co-glycolide-co-caprolactone) (PLGA-PCL) nanoparticles (NPs) capable of sustained release of MMP-1. We established quadratic equations as mathematical models and employed rotatable central composite design and response surface methodology to optimize the preparation procedure of the NPs. Then, characterization of the optimized NPs with respect to particle size distribution, particle morphology, drug encapsulation efficiency, MMP-1 activity assay and in vitro release of MMP-1 from NPs was carried out. The results of mathematical modeling show that the optimal conditions for the preparation of MMP-1-loaded NPs were as follows: 7 min for the duration time of homogenization, 4.5 krpm for the agitation speed of homogenization and 0.4 for the volume ratio of organic solvent phase to external aqueous phase. The entrapment efficiency and the average particle size of the NPs were 38.75 ± 4.74% and 322.7 ± 18.1 nm, respectively. Further scanning electron microscopy image shows that the NPs have a smooth and spherical surface, with mean particle size around 300 nm. The MMP-1 activity assay and in vitro drug release profile of NPs indicated that the bioactivity of the enzyme can be reserved where the encapsulation allows prolonged release of MMP-1 over 60 days. Taken together, we reported here novel PLGA-PCL NPs for sustained release of MMP-1, which may provide an ideal MMP-1 delivery approach for tissue reconstruction therapy.     

Statistical optimization for biodiesel production from waste frying oil through two-step catalyzed process

The aim of this work was to investigate the optimum conditions in biodiesel production from waste frying oil using two-step catalyzed process. In the first step, sulfuric acid was used as a catalyst for the esterification reaction of free fatty acid and methanol in order to reduce the free fatty acid content to be approximate 0.5%. In the second step, the product from the first step was further reacted with methanol using potassium hydroxide as a catalyst. The Box-Behnken design of experiment was carried out using the MINITAB RELEASE 14, and the results were analyzed using response surface methodology. The optimum conditions for biodiesel production were obtained when using methanol to oil molar ratio of 6.1:1, 0.68 wt.% of sulfuric acid, at 51 °C with a reaction time of 60 min in the first step, followed by using molar ratio of methanol to product from the first step of 9.1:1, 1 wt.% KOH, at 55 °C with a reaction time of 60 min in the second step. The percentage of methyl ester in the obtained product was 90.56 ± 0.28%. In addition, the fuel properties of the produced biodiesel were in the acceptable ranges according to Thai standard for community biodiesel.     

纳米氧化镍的制备与应用

纳米氧化镍具有优异的催化性能、电学性能,在催化剂、传感器及电池电极等方面得到了广泛的应用。综述了纳米氧化镍的制备方法及其优缺点,指出了纳米氧化镍在制备及其表面改性方面尚待解决的问题。     

Uneven distribution of nanoparticles in immiscible fluids: Morphology development in polymer blends

The present review aims at summarizing the current knowledge on how solid nanoparticles organize in polymer blends. First, the behavior of low viscosity fluid emulsions containing solid colloidal particles is briefly presented. By contrast with polymer blends, they have been the subject of intensive studies for a long time, with both applicative and comprehensive objectives. High viscosity fluid emulsions like polymer blends loaded with nanofillers have received less attention until the recent enthusiasm about nanotechnology and more specifically polymer nanocomposites. Some similarities and differences between both types of emulsions are highlighted. The solid particles are well known to distribute unevenly in those types of complex fluids and the factors that determine their distribution in polymer blends are discussed. A particular emphasis is given on the competition between thermodynamic wetting of the solid by the polymeric phases and kinetic control of the filler localization directly linked to the rate of the mixing process. This aspect is believed to be a specificity of filled polymer blends and is known to have a drastic and sometimes predominant effect on particle localization. It explains that finely tuned morphologies can be obtained where the particles do not occupy their equilibrium position.     

Box-Behnken实验设计法优化厚朴酚与和厚朴酚的提取工艺

优化厚朴中厚朴酚与和厚朴酚的提取工艺。选用厚朴酚与和厚朴酚的总收率为响应值,采用四因素三水平的Box-Behnken实验设计,对影响厚朴酚、和厚朴酚提取的主要因素进行考察,建立相应的二项式数学模型优化提取工艺。最优工艺条件是乙醇浓度为65%,提取液p H值为9.5,提取时间为65.2min,液料比(乙醇体积与厚朴质量比,m L/g)为8.04。Box-Behnken实验设计法可用于厚朴酚与和厚朴酚提取工艺的优化。     

Experimental design and batch experiments for optimization of Cr(VI) removal from aqueous solutions by hydrous cerium oxide nanoparticles

Hydrous cerium oxide (HCO) was synthesized by intercalation of solutions of cerium(III) nitrate and sodium hydroxide and evaluated as an adsorbent for the removal of hexavalent chromium from aqueous solutions. Simple batch experiments and a 2⁵ factorial experimental design were employed to screen the variables affecting Cr(VI) removal efficiency. The effects of the process variables; solution pH, initial Cr(VI) concentration, temperature, adsorbent dose and ionic strength were examined. Using the experimental results, a linear mathematical model representing the influence of the different variables and their interactions was obtained. Analysis of variance (ANOVA) demonstrated that Cr(VI) adsorption significantly increases with decreased solution pH, initial concentration and amount of adsorbent used (dose), but slightly decreased with an increase in temperature and ionic strength. The optimization study indicates 99% as the maximum removal at pH 2, 20 °C, 1.923 mM of metal concentration and a sorbent dose of 4 g/dm³. At these optimal conditions, Langmuir, Freundlich and Redlich–Peterson isotherm models were obtained. The maximum adsorption capacity of Cr(VI) adsorbed by HCO was 0.828 mmol/g, calculated by the Langmuir isotherm model. Desorption of chromium indicated that the HCO adsorbent can be regenerated using NaOH solution 0.1 M (up to 85%). The adsorption interactions between the surface sites of HCO and the Cr(VI) ions were found to be a combined effect of both anion exchange and surface complexation with the formation of an inner-sphere complex.     

纳米羟基磷灰石的制备及表征

采用化学沉淀法制备了羟基磷灰石纳米粒子,并且通过扫描电子显微镜(SEM)、X射线衍射(XRD)、红外光谱(IR)等测试手段,对其进行了表征。实验结果表明:以Ca(OH)2和H3PO4为原料所制备出的纳米羟基磷灰石纳米粒子多呈针状或短棒状,平均粒径20~25 nm,长75~80 nm,且大小均匀,分散性好。尺寸和形状更接近人体骨磷灰石结构,并能与骨形成牢固的化学结合,是一种很有应用前景的人工骨和人工口腔材料。     

CO铜基变换催化剂氰化氢中毒机理热力学研究

为了掌握CO变换催化剂在高炉煤气气氛下的中毒机理,文中采用热力学非均相反应体系中的Gibbs自由能最小原理,从理论上分析了CO变换催化剂在高炉煤气气氛下,HCN中毒可能发生的化学反应及产物。对各个反应的吉布斯自由能及化学反应平衡常数进行了对比分析,结果表明:氰化氢(HCN)对于铁基高温变换催化剂在其活性温度下的中毒作用很小,而对于铜基低温变换催化剂在100—300℃的活性温度下,主要的中毒产物为CuCN,CuO,Cu2O,Cu(OH)2,C,且高炉煤气自身的主要气体混合也是使催化剂中毒的原因之一。此外,氧气的存在会加快催化剂的中毒反应。其中低温变换催化剂的活性物质Cu微晶与CO和O2反应的吉布斯自由能小于0,且绝对值最大,热力学平衡常数最大。这个反应是竞争能力最强的主导反应。     

A flame metal combustion method for production of nanoparticles

We propose a flame metal combustion method for continuously synthesizing metal oxide nanoparticles. Micro-sized metal powder precursors were injected into a hydrogen-oxygen flame through a newly designed feeder system in order to be completely converted into metal oxide nanoparticles with good crystallinity. There is no limitation in the selection of precursors including metal, metal chloride and metal organic powders to synthesize nanoparticles. Various oxides such as magnesia, iron oxides and zinc oxide were demonstrated to be successfully generated by using this method. The sizes of oxide nanoparticles were controlled by varying flame temperatures and residence times.     

Fluidization of nanoparticles: A simple equation for estimating the size of agglomerates

In this work, we revise data published in the last decade on the size of agglomerates in gas-fluidized beds of nanoparticles. Experimental measurements reviewed are based on non-invasive techniques, mainly consisting of laser-based planar visualization of agglomerates in the splash zone and indirect derivation from the fit of bed expansion, settling, and/or minimum fluidization velocity data to empirical correlations. Special attention is focused on the effect of fluidization aids such as vibration, magnetic assistance, sound excitation or centrifugation. Independent measurements performed by diverse authors or by the same authors using different techniques are confronted. Empirical models proposed to predict agglomerate size are also reviewed. Most of these models are difficult to apply in practice because they rely on parameters that need to be measured in the fluidization experiment or assumed. We propose a simple equation to estimate agglomerate size derived from the balance between the local shear force on the particle attached at the outer layer of the agglomerate and the interparticle adhesion force. In general, the results predicted by this equation are in satisfactory agreement with the reviewed experimental data.     

Using a glowing wire generator for production of charged, uniformly sized nanoparticles at high concentrations

The glowing wire represents a clean method of producing particles from a few nanometers to some tens of nanometers in diameter. An empirical rule is derived, identifying the materials, for which the method is applicable. A fraction of the particles is already charged at an efficiency comparable to radioactive chargers. This allows the direct use for mobility size classification and deposition without any further charging step. By applying a potential difference to the wire with respect to the housing, the charged particle yield can be increased by almost two orders of magnitude. Downstream of a mobility classifier a maximum concentration as high as was reached. The generator shows excellent long-term stability.     

全钢载重子午线轮胎胎肩垫胶配方优化设计

本试验对全钢载重子午线轮胎胎肩垫胶配方进行优化设计。结果表明：通过配方优化,提高胎肩垫胶配方的含胶率,调整硫化体系并使用抗硫化返原剂,降低了胎肩垫胶的生热,提高了疲劳寿命,提高了轮胎的高速、耐久性能,改善了肩空、肩裂质量问题。     

Preparation of goat milk powder with Lactobacillus casei L61 and antioxidant peptides: optimization of the composite thermal protectants and evaluation of storage stability

Abstract

The Lactobacillus casei L61 has great ability for producing antioxidant peptides. For reducing the mortality of L. casei L61 in spray drying process, the Box-Behnken design (BBD) was adopted to optimize the composite thermal protective agent formula. The results exhibited that the composite thermal protective agent formula of L. casei L61 contained glucose at 6.03% (w/v), skim milk at 18.98?g/L, and glycerol at 12.50?mL/L. Under the optimal conditions, the average survival of L. casei L61 in the fermented goat milk reached 14.58?±?0.72% after heat treatment at 75?°C for 10?min, which was higher than the control (13.14%). The average hydroxyl free radical scavenging activity of L. casei L61 reached 85.09?±?0.98%, which was not significantly different from the predicted value (86.83%). Therefore, the BBD is feasible for optimizing the composite thermal protective agent formula of L. casei L61. Under the optimal conditions with the inlet air temperature of 130?°C and feed rate of 4.5?mL/min, the maximum viable counts and survival rate of L. casei L61 were 7.46?×?10⁸ cfu/g and 23.41?±?1.28%, respectively. More importantly, the storage stability of antioxidative probiotic goat milk powder was predicted by temperature acceleration test. The shelf life of antioxidative probiotic goat milk powder was estimated to be 352?days at 4?°C and 117?days at 25?°C, embodying the great long-term stability. This study provides a technical reference for industrialized production of probiotic goat milk powder.     

Synthesis and application of lead telluride nanoparticles for degrediation of organic pollution

PbTe nanoparticles were achieved from reaction of Pb(NO)₃ and TeCl₄ (as a new precursor for Tellur) in a relatively short time and low temperature in a hydrothermal process. The photocatalytic behavior of nanoparticles was evaluated using the degradation of a methyl orange (MeO) aqueous solution (as an organic pollution) under ultraviolet (UV) light irradiation. The results confirm that nanoparticles are promising materials with excellent performance in photocatalytic applications. In addition to, observations suggest that the as-obtained PbTe nanoparticles exhibit a strong PL peak at room temperature that might be ascribed to the high level transition in the PbTe semiconductor.     

Structure and catalytic activity of POSS-stabilized Pd nanoparticles

Palladium nanoparticles stabilized with polyhedral oligomeric silsesquioxanes have been characterized and determined to function as a heterogeneous catalyst. TEM and SEM studies indicate the material comprises 2–5 nm diameter Pd crystallites in a POSS layer, which aggregate to form spherical secondary structures of about 50 nm in diameter. Solid-state NMR reveals that the primary interaction between Pd and POSS is through the alkyl-amino functional groups on the POSS cage, in addition to some weak interactions with the cage itself. This material is observed by microbalance measurements to efficiently catalyze the direct hydrogenation of 1,4-diphenylbutadiyne.     

Tin oxide nanoparticles synthesized by gel combustion and their potential for gas detection

Tin oxide nanoparticles were synthesized starting from SnCl₄·5H₂O with the aid of polyacrylamide gel. The pyrolysis of the gel and the influence of the calcination temperature were discussed based on thermogravimetric analysis and X-ray powder diffraction. The decomposition of the polyacrylamide gel occurred mainly in the temperature range of 220–600 °C, after which resulting in a heap of fine powders. The average grain size of the nanoparticles synthesized at 600, 700 and 800 °C were calculated to be 8.1, 19.2 and 27.9 nm, respectively. The prepared SnO₂ nanoparticles were sphere-like and uniform in size, weakly aggregated in thin platelets as indicated by scanning electron microscope (SEM) images. Thick-film sensor samples based on the as-synthesized SnO₂ nanoparticles without specific additives showed response sensitivity of around 28.8 at the optimal detection temperature of 150 °C to 30 ppm H₂S gas, while their responses to 1000 ppm of CO or CH₄ were negligible.