Azeotropic behaviour of (benzene + cyclohexane + chlorobenzene) ternary mixture using chlorobenzene as entrainer at 101.3 kPa

In this paper, the azeotropic behaviour of the (benzene + cyclohexane + chlorobenzene) ternary mixture was experimentally investigated with the aim of enhancing the knowledge for the feasible use of chlorobenzene as an entrainer for the azeotropic distillation of the binary azeotrope. Such a study has not been reported in the literature to the best of the authors’ knowledge. (Vapour + liquid) equilibria data for (benzene + cyclohexane + chlorobenzene) at 101.3 kPa were obtained with a Othmer-type ebulliometer. Data were tested and considered thermodynamically consistent. The experimental results showed that this ternary mixture is completely miscible and exhibits an unique binary homogeneous azeotrope, an unstable node at the conditions studied, and the propitious topological characteristics (residual curve map and relative volatility) to be separated. Satisfactory results were obtained for the correlation of equilibrium compositions with the UNIQUAC activity coefficients model and also for prediction with the UNIFAC method. In both cases, low root mean square deviations of the vapour mole fraction and temperature were calculated. The capability of chlorobenzene as a modified distillation agent at atmospheric condition is discussed in terms of the thermodynamic topological analysis. A conceptual distillation scheme with reversed volatility is proposed to separate the azeotropic mixture. In order to reduce the operational cost requirements of the sequence of columns proposed, the range for optimal reflux and the ratio for feed flow conditions were studied.     

超临界CO_2萃取板蓝根靛玉红的工艺优化研究

采用正交试验法,对板蓝根靛玉红超临界CO2萃取工艺进行优化。选用萃取温度、萃取压力、萃取时间作为正交试验的3个因素,每个因素选3个水平,以提取物中靛玉红的含量来确定最佳提取条件,并且在最佳条件下确定所加夹带剂的最佳剂量。结果表明最佳工艺为:萃取温度45℃、萃取压力35MPa、萃取时间3h,夹带剂为75%的乙醇200mL。最佳工艺条件下提取靛玉红的得率为4.95μg/g,为传统提取方法的1.6倍。     

Effects of processing parameters in the sonic assisted water extraction (SAWE) of 6-gingerol

The use of water in subcritical conditions for extraction has several drawbacks. These include the safety features, higher production costs and possible degradation of the bioactive compounds. To overcome these problems, sonic energy and an entrainer were used as external interventions to decrease the polarity of water at milder operating conditions. The effect of low (28 kHz) and high (800 kHz) frequencies of sonication in the extraction of the main ginger bioactive compound (6-gingerol) were compared. Six parameters were studied: mean particle size (MPS, mm), time of extraction, applied power, sample to solvent ratio (w/v), temperature of extraction, and the percentage of entrainer. The optimum conditions for high frequency SAWE prototype were MPS 0.89–1.77 mm, 45 min, 40 W applied power, 1:30 (w/v), 45 °C, and 15% of ethanol as entrainer. Two-way analysis of variance (ANOVA) gave the most significant parameter, which was power with F (1, 45.07), p < 2.50 × 10⁻⁹. Although the effect of low frequency was stronger than high frequency, at the optimum conditions of the sample to solvent ratio 1:30 (w/v) with 700 mL solvent and temperature 45 °C, the concentration and recovery of 6-gingerol from high frequency of SAWE prototype was 2.69 times higher than at low frequency of SAWE. It was found that although the effects of high frequency (800 kHz) were negligible in other studies, it could extract suitable compounds, such as 6-gingerol, at lower temperature. Therefore, the effects of sonication, which cause an enlargement in the cell wall of the ginger plant matrix, were observed using a Scanning Electron Microscope (SEM). It was found that the applied power of sonication was the most significant parameter compared to the other parameters.     

Vapor-liquid equilibria of ternary systems with 1-ethyl-3-methylimidazolium ethyl sulfate using headspace gas chromatography

Vapor-liquid equilibria (VLE) for two binary systems 1-propanol + water and methyl acetate + methanol, and the ternary mixtures with the ionic liquid 1-ethyl-3-methylimidazolium ethyl sulfate [EMIM]⁺[EtSO₄]⁻ as entrainer were measured by headspace gas chromatography. From the experimental VLE data, the influence of the ionic liquid on the separation factors was investigated. The experimental results for the ternary systems show that [EMIM]⁺[EtSO₄]⁻ has a great influence on the separation factors of the systems investigated. Furthermore, the experimental separation factors were compared with the predicted ones of other ionic liquids and conventional selective solvents using modified UNIFAC (Dortmund).     

Entrainer effect in supercritical mixtures

The objective of this paper is to propose a predictive method for the estimation of the change in the solubility of a solid in a supercritical solvent when another solute (entrainer) or a cosolvent is added to the system. To achieve this goal, the solubility equations were coupled with the Kirkwood–Buff (KB) theory of dilute ternary solutions. In this manner, the solubility of a solid in a supercritical fluid (SCF) in the presence of an entrainer or a cosolvent could be expressed in terms of only binary data. The obtained predictive method was applied to six ternary SCF–solute–cosolute and two SCF–solute–cosolvent systems. In the former case, the agreement with experiment was very good, whereas in the latter, the agreement was only satisfactory, because the data were not for the very dilute systems for which the present approach is valid.     

超临界二氧化碳二元体系相平衡性质的研究

采用固定体积可视观察法测定了CO₂+甲苯、CO₂+环己烷、CO₂+正丁醛、CO₂+异丁醛、CO₂+甲醇及CO₂+乙醇二元体系的临界点性质,为超临界萃取和化学反应提供基础数据.在对二元体系相行为与单组分超临界相行为进行比较的基础上,对不同化学物质及不同配比的二元体系临界点与二氧化碳临界点之间的关系进行了讨论.