Alkoxyl side-chain effects of acidic ionic liquids catalysts for the esterification of n-butyl butyrate

Three kinds of alkoxy group-functionalized acidic ionic liquids (ILs) are reported in this work, namely, 1-(methoxyethyl)-3-methylimidazolium hydrogen sulphate [MOE-MIM]HSO₄, 1-(ethyoxyethyl)-3-methylimidazolium hydrogen sulphate [EOE-MIM]HSO₄, and 1-(propyoxyethyl)-3-methylimidazolium hydrogen sulphate [POE-MIM]HSO₄. The short side chain on the cation of [MOE-MIM]HSO₄ decreases the solubility of the IL in butanol and butyric acid and facilitates the separation of the IL from a reaction medium. The yield of butyl butyrate is up to 99.5%. After 10 rounds of recycling, the catalytic performance of [MOE-MIM]HSO₄ shows no significant changes.     

Transient liquid phase sintering of high-purity mullite for high-temperature structural ceramics

High-purity mullite ceramics, promising engineering ceramics for high-temperature applications, were fabricated using transient liquid phase sintering to improve their high-temperature mechanical properties. Small amounts of ultrafine alumina or silica powders were uniformly mixed with the mullite precursor depending on the silica-alumina ratio of the resulting ceramics to allow for the formation of a transient liquid phase during sintering, thus, enhancing densification at the early stage of sintering and mullite formation by the reaction between additional alumina and the residual glassy phase (mullitization) at the final stage of sintering. The addition of alumina powder to the silica-rich mullite precursor resulted in a reaction between the glassy silica and alumina phases during sintering, thereby forming a mullite phase without inhibiting densification. The addition of fine silica powder to the mullite single-phase precursor led to densification with an abnormal grain growth of mullite, whereas some of the added silica remained as a glassy phase after sintering. The resulting mullite ceramics prepared using different powder compositions showed different sintering behaviors, depending on the amount of alumina added. Upon selecting an optimum process and the amount of alumina to be added, the pure mullite ceramics obtained via transient liquid phase sintering exhibited high density (approximately 99%) and excellent high-temperature flexural strength (approximately 320 MPa) at 1500 °C in air. These results clearly demonstrate that pure mullite ceramics fabricated via transient liquid phase sintering with compositions close to those of stoichiometric mullite could be a promising process for the fabrication of high-temperature structural ceramics used in an ambient atmosphere. The transient liquid phase sintering process proposed in this study could be a powerful processing tool that allows for the preparation of superior high-temperature structural ceramics used in the ambient processing atmosphere.     

Charge Transportation and Chirality in Liquid Crystalline Helical Network Phases of Achiral BTBT-Derived Polycatenar Molecules

First examples of multichain (polycatenar) compounds, based on the π-conjugated [1]benzothieno[3,2-b]benzothiophene unit are designed, synthesized, and their soft self-assembly and charge carrier mobility are investigated. These compounds, terminated by the new fan-shaped 2-brominated 3,4,5-trialkoxybenzoate moiety, form bicontinuous cubic liquid crystalline (LC) phases with helical network structure over extremely wide temperature ranges (>200 K), including ambient temperature. Compounds with short chains show an achiral cubic phase with the double network, which upon increasing the chain length, is at first replaced by a tetragonal 3D phase and then by a mirror symmetry is broken triple network cubic phase. In the networks, the capability of bypassing defects provides enhanced charge carrier mobility compared to imperfectly aligned columnar phases, and the charge transportation is non-dispersive, as only rarely observed for LC materials. At the transition to a semicrystalline helical network phase, the conductivity is further enhanced by almost one order of magnitude. In addition, a mirror symmetry broken isotropic liquid phase is formed beside the 3D phases, which upon chain elongation is removed and replaced by a hexagonal columnar LC phase.     

堆本体抗震试验动力相似关系推导与验证

为确保堆本体抗震试验中流体对流效应、脉冲效应和堆本体结构响应的准确性，需保证重力、流体与固体惯性力、结构弹性力和结构应变的相似性。本文从固体结构的振动方程、不可压牛顿流体的动力学方程、流固交界面的边界条件和环形柱体域内液体线性晃动的动力学公式出发，基于控制方程的量纲分析法，推导了考虑液体晃动效应的堆本体地震响应动力相似关系。基于上述相似关系建立了堆容器堆内构件和堆容器内自由液面流体域的缩尺模型，通过有限体积法分析堆容器堆内构件原型和缩尺模型中液体的晃动固有频率、晃动波高、压力以及液体晃动对堆容器支承裙的倾覆力矩。结果表明本文动力相似关系具有合理性和准确性，可用于堆本体缩尺模型的抗震试验研究。     

超高效液相色谱-飞行时间质谱法快速分析测定山药中7种常见杀菌剂

目的 建立超高效液相色谱-飞行时间质谱检测山药中7种常见杀菌剂的分析方法。方法 样品经乙腈提取，水浴氮吹至近干，丙酮定容，经超高效液相色谱-飞行时间质谱检测。结果 在正离子模式下，7种杀菌剂在水-甲醇（均含有0.01%甲酸和5 mmol/L甲酸铵）流动相中都具有较好的响应；0.01~0.40 mg/L范围内线性良好，相关系数R均大于0.999。不同温度（50℃、70℃）水浴实验结果表明70℃水浴温度符合实验要求。三个浓度水平的加标回收实验的回收率为70.75％～108.07％，相对标准偏差为 0.02％～5.01％。结论 该方法操作简单、分析准确，满足山药中常见杀菌剂的检测要求。     

超高效液相色谱-串联质谱法同时检测糕点中6种甜味剂

目的建立超高效液相色谱-串联质谱法同时测定糕点中6种常用合成甜味剂的分析方法。方法选用超纯水作为提取溶剂,涡旋和超声提取后,低温离心,取部分上清液加入正己烷除脂,Waters Atlantis■T3色谱柱、甲醇-5 mmol/L甲酸铵(含0.1%甲酸)作为流动相、亲水亲脂平衡型固相萃取柱HLB(hydrophile-lipophile balance)净化。结果6种甜味剂在质量浓度为10~200 ng/mL的曲线范围内呈良好线性关系,相关系数r均大于0.999,平均加标回收率在85.0%-98.2%之间,相对平均偏差(relative standard deviation,RSD)为1.3%~6.7%。结论该方法具有前处理简单、灵敏度高、检测速度快等优点,适合糖精钠、甜蜜素、三氯蔗糖、阿斯巴甜、阿力甜、纽甜的检测,但不适用于安赛蜜的检测。     

Producing Fatty Acid Methyl Esters from Free Fatty Acids with Ionic Liquids as Catalyst

Three Brønsted acidic imidazole dicationic ionic liquids (ILs) with different length of alkyl chains, [C_n(Mim)₂][HSO₄]₂ (n = 3, 6, 12), were prepared and used as catalyst for the esterification reaction of free fatty acids and methanol. Taking oleic acid as model acid, the catalytic performances of the synthesized ILs for the esterification were evaluated. The main physicochemical properties of the ILs, thermal stability, acidity, solubility in common solvents, and causticity on Austenitic stainless steel 316, were examined. [C₃(Mim)₂][HSO₄]₂ demonstrated the highest catalytic activity and enabled to assess the preliminary optimum esterification condition of oleic acid and methanol. Under optimized reaction conditions, the yield of oleic acid methyl ester was up to 95 %. The ILs have great potential as catalysts for producing fatty acid methyl esters from long‐chain free fatty acids.     

Analysis of the water-soluble compounds as a tool for discriminating traditional and industrial high moisture mozzarella made with citric acid

High moisture mozzarella from cow milk is a pasta filata cheese that can be manufactured by different protocols. Fermentation by autochthonous starter is used for the traditional product, whereas direct acidification with citric acid is widely used at industrial level. Both types are stored immersed in a liquid for preserving freshness, but this packaging method is known to favour the changes of the quality characteristics. The present study aimed to assess the evolution of the soluble compounds and to evaluate their use as chemical indices for discriminating the two types of mozzarella. The contents of lactose, organic acids, water-soluble nitrogen and free amino acids differently changed over time. The whole patterns of these soluble compounds allowed discrimination of the two products during the whole storage period. The simple analyses of lactic acid and lactose could be a rapid tool to protect traditional mozzarella from industrial imitations obtained with citric acid.     

Experimental study on prediction model of wet gas pressure drop across single-orifice plate in horizontal pipes in the low gas phase Froude number region

The pressure drop prediction of wet gas across single-orifice plate in horizontal pipes had been solved satisfactorily under an annular-mist flow in the upstream of orifice plates. However, this pressure drop prediction is still not clearly determined when the upstream is in an intermittent flow or stratified flow, which is corresponding to a region of low Fr_G (gas phase Froude number) in the flow pattern map of wet gases. In this study, the wet gas pressure drop across a single-orifice plate was experimentally investigated in the low Fr_G region. By the experiment, the flow pattern transition in the downstream of single-orifice plates, as well as the effects of Fr_G and Fr_L (liquid phase Froude number) on Φ_G (gas phase multiplier), were determined and compared when the upstream is in the flow pattern transition and the stratified flow region, respectively. Prediction performances were examined on the available pressure drop models. It was found that no model could be capable of jointly predicting the wet gas pressure drop in the low Fr_G region with an acceptable accuracy. With a new method of correlating Fr_G and Fr_L simultaneously, new correlations were proposed for the low Fr_G region. Among which the modified Chisholm model shows the best prediction accuracies, with the prediction deviations of Φ_G being within 7% and 3% when the upstream is in flow pattern transition and stratified flow region, respectively.     

月桂酰肌氨酸钠搭建阿尔法凝胶的方法研究及结构表征

阿尔法凝胶作为一种特殊的液晶结构，能够在清洁或调理皮肤的过程中给皮肤毛发提供更好的湿润感和调理性。由于阿尔法凝胶结构的搭建传统方法需要不少于14个碳原子的烷基表面活性剂，其实际应用一直受到限制。提供了一种由月桂酰肌氨酸钠作为烷基碳链为12个碳原子的氨基酸型表面活性剂搭建阿尔法凝胶的方法，并对其产物进行结构表征和分析。