酮麝香-二甲苯麝香双液相萃取结晶

To evaluate the effect of two liquid phase on the separation of musks mixture, the phase equilibria of musk ketone musk xylene dimethyl sulfoxide heptane system were studied for the first time. The whole and every part of the phase equilibrium for the quaternary system were shown by three-dimensional phase diagrams, the liquid-liquid equilibria, solid-liquid equilibria and solid-liquid-liquid equilibria of the quaternary system were also shown. As a result, the compositions of musks in the equilibrium liquid phases were different from those in the feed, that is, musk ketone was enriched in dimethyl sulfoxide phase while musk xylene was enriched in heptane phase. So these equilibrium liquid phases were useful in separating musk ketone and musk xylene. On the basis of these results, a new process “two liquid phase extractive crystallization” was proposed to separate the eutectics of musk ketone and musk xylene.     

UNIFAC模型法计算含己内酰胺体系的相平衡(英文)

An extended liquid-liquid equilibrium (LLE) UNIFAC model is proposed to describe phase equilibria of mixtures containing caprolactam. In this model, caprolactam is introduced as a new group. New group interaction parameters are calibrated from 156 sets of liquid-liquid equilibrium data. The present model gives satisfactory correlation and prediction in liquid-liquid equilibrium, including quaternary systems containing the mixed solvent of an alcohol and an alkane. The model can be applied to predict caprolactam solubility in water and benzene accurately. Freezing point and vapor-liquid equilibrium of binary systems containing caprolactam are also predicted with the extended LLE UNIFAC model. Satisfactory prediction results are obtained.     

Solid-liquid equilibrium of dimethyl terephthalate(DMT),dimethyl isophthalate(DMI)and dimethyl phthalate(DMP)in melt crystallization process

The binary solid-liquid equilibrium of Dimethyl Terephthalate(DMT),Dimethyl Isophthalate(DMI)and Dimeth-yl Phthalate(DMP)was investigated by experiment and differential scanning calorimetry(DSC).The result dem-onstrated DMT/DMI and DMT/DMP systems are eutectic while DMI/DMP is a solid-solution system.The eutectic temperature of DMT/DMI system is 336.7 K and that of DMT/DMP is 271.1 K.Furthermore,a classical solid-liquid phase equilibrium model was used to fit the experimental data of the eutectic systems of DMT/DMI and DMT/DMP and the theoretical model could describe the eutectic solid-liquid phase diagrams properly.     

酮麝香，二甲苯麝香溶液结晶研究

1 INTRODUCTION Musk ketone and musk xylene are important syn- thetic nitro-musks. They are high boiling substances and subject to decomposition under the condition of heat and light. When they are melted, the liquid mix- ture is very sticky, which lead to high resistance to heat and mass transfer and difficulty in solidification. As a result, it is reasonable to employ solution crys- tallization to separate and purify musk mixture. As the basis of solution crystallization, the solubility …     

基于UNIFAC模型的基团-OCOO-与-CH3,ACH,CH3OH和CH3COO-的交互作用参数估算与验证

Isobaric vapor-liquid equilibria (VLE) are experimentally measured for the binary systems of dimethyl carbonate (DMC) ethylene carbonate and methanol ethylene carbonate at 101.325kPa. The thermodynamic consistency of these experimental data is tested with an available statistic method. Interaction parameters of the carbonate group —OCOO— with the group —CH3, ACH, CH3OH and CHACO0— in UNIFAC model are determined using the experimental and literature VLE data. The results show that the calculated VLE data using the new UNIFAG parameters agree excellently with the experimental data in this work and in literature. These results are useful in the research on DMG and diphenyl carbonate synthesis by transesterification in design of reactor and distillation tower.     

顺丁烯二酸酐在单一溶剂和混合溶剂中的固液平衡研究

Solid-liquid equilibria (SLE) of three binary systems and seven ternary systems containing maleic anhydride(MA) are measured by visual method. The experimental data are compared with the calculated ones with modified universal quasichemical functional group activity coefficient(UNIFAC) method in which the interaction parameters between groups come from two sources, dortmund data bank(DDB), if there’s any, and correlations based on our former presented experimental SLE data of twenty binary systems. New groups of MA, ACCOO group, COO group, ＞C=O group and cy-CH2 group are defined and the SLE data of maleic anhydride in isopropyl acetate in literature are cited in order to assess the new interaction parameters, correlated with Wilson equation and the λh equation. The modified UNIFAC method with these new regressed interaction parameters is also used to predict other three binary systems containing maleic anhydride.     

Solid-Liquid Equilibria of Several Binary and Ternary Systems Containing Maleic Anhydride

Solid-liquid equilibria (SLE) of three binary systems and seven ternary systems containing maleic an-hydride(MA) are measured by visual method. The experimental data are compared with the calculated ones with modified universal quasichemical functional group activity coefficient(UNIFAC) method in which the interaction parameters between groups come from two sources, dortmund data bank(DDB), if there's any, and correlations based on our former presented experimental SLE data of twenty binary systems. New groups of MA, ACCOO group, COO group, >C=O group and cy-CH2 group are defined and the SLE data of rnaleic anhydride in isopropyl acetate in literature are cited in order to assess the new interaction parameters, correlated with Wilson equation and the λh equation. The modified UNIFAC method with these new regressed interaction parameters is also used to predict other three binary systems containing rnaleic anhydride.     

苯或甲苯萃取己内酰胺和甲基己内酰胺分配系数的测定和预测

To get high purity caprolactam is a challenging task in the chemical fiber industry. To date, reports on the prediction of the distribution of caprolactam and its derivative chemicals have been few. In this study, the ex-traction of caprolactam with toluene as the extractant and N-methyl caprolactam with benzene and toluene as the extractants has been carried out. By defining new UNIFAC groups and calibrating related interaction parameters, a UNIFAC method was introduced to predict the equilibrium concentration of caprolactam and methyl caprolactam in toluene or benzene extraction processes. The calculated results fit very well with the experimental data. Using the UNIFAC model, the selectivity of extractants can be predicted.     

甲基-酰基-萘在庚烷、辛烷和十二烷中溶解度的测定与关联

The solubilities of 2-methyl-6-acetylnaphthalene (2,6-MAN) and 2-methyl-7-acetylnaphthalene (2,7-MAN) in n-heptane, n-octane, and n-dodecane were measured, respectively, from 273.15 to 319.15K using an analytical method. On the basis of the thermodynamics theory of solid-liquid equilibrium, a model was derived to relate the solubilities with temperature. Using the least square method, the parameters of the model, the fusion enthalpies ΔfusH and the Margules equation coefficients A12 and A21 of 2,6-MAN and 2,7-MAN in n-heptane, n-octane, and n-dodecane—were obtained by regressing the experimental data. The average deviation of the model was 1.70%.     

戊二酸在冰醋酸和环己酮、环己醇及五种混合溶剂中的溶解度的测定

By using the laser-monitoring technique, solid-liquid equilibrium data of glutaric acid in cyclohexanol, cyclohexanone, their five mixed solvents and acetic acid were measured within the temperature range from 292.15K to 354.60K by dynamic method. Empirical formula and λh equation were used to correlate the solubilities of glutaric acid in eight solvents. The maximal average relative deviations were 1.15% and 2.20% by using the empirical formula and λh equation to correlate the solubility data. The results showed that the empirical formula and λh model could correlate the solubility data of glutaric acid in eight solvents. In addition, the solubility data of glutaric acid in five mixtures （cyclohexanone＋cyclohexanol） could be predicted with the NRTL equation utilizing the parameters of the binary systems. The total average relative deviation was 3.60%. The results indicate that the NRTL equation could well predict the solubilities of glutaric acid in the mixed solvents of cyclohexanone and cyclohexanol.     

酮麝香、二甲苯麝香和双溶剂四元体系液液相平衡研究

本文计算并测定了酮麝香、二甲苯麝香、二甲基亚砜(或乙腈)和庚烷(或环己烷)四元体系的液液相平衡,试验结果与计算值基本吻合。平衡双液相中两种麝香的比例不同于原料,两液相中两种麝香分别得到了富集,其中二甲基亚砜(或乙腈)相中富含酮麝香、庚烷(或环己烷)相中富含二甲苯麝香,这种液相分相可用于分离麝香混合物。本文的研究为麝香混合物的分离提供了理论指导。此外,采用本文的方法还可以预测较难测定的多元固、液混合物的相平衡关系。     

麝香体系结晶分离研究

研究了根据酮麝香、1,3-二甲基-2,4-二硝基-5-叔丁基苯晶体生长速度的不同,从对二者均达到饱和的溶液中分离得到1,3-二甲基-2,4-二硝基-5-叔丁基苯晶体的过程,计算了晶体生长速度并进行了实验验证。     

含麝香体系多元溶液固液平衡研究

测定了酮麝香、二甲苯麝香在单一溶剂和混合溶剂中的溶解度以及酮麝香的中间体 2 ,6 二甲基 4 叔丁基苯乙酮在不同溶剂中的溶解度 ,并且测定了多溶质多溶剂体系的固液平衡 ,采用UNIFAC活度系数法进行以上体系的固液平衡计算 ,计算结果与实验测定结果吻合良好。采用文中提出的方法不仅可以预测多溶质体系在溶液中共同达到饱和时的溶解度 ,而且可以预测部分溶质达到饱和时的溶解度 ,这对于溶液结晶具有重要的指导意义     

UNIFAC基团贡献法对合成硝基麝香固液平衡的研究

应用UNIFAC基团贡献法研究了合成硝基麝香物系在乙酸乙酯、乙腈、环己烷等溶剂中的溶解度。通过麝香物系在多种溶剂中的二元相平衡的实验数据对UNIFAC交互作用参数进行了回归修正,并利用这些交互作用参数预测了大量麝香的二元、三元的固液平衡,与实验值比较,证明参数修正的结果是理想的,误差在允许范围之内,能满足合成硝基麝香体系固液平衡计算的需要。     

合成麝香双液相萃取结晶溶剂研究

对组分处于低共熔点的麝香体系提出了一种新的萃取方法———双液相萃取结晶。利用修正的UNIFAC模型对麝香在不同溶剂中的平衡数据进行预测,根据相平衡数据对各种溶剂进行比较,从理论上筛选出麝香体系合适的萃取溶剂,再进行实验验证。结果表明,麝香混合物在加入2种溶剂(乙腈+环己烷)完全溶解后,出现明显的分相,在不同的相中麝香的比例均比初始比例发生了很大的变化,得到了理想的富集,这样就使每种麝香更容易分离。     

长碳链二元酸在人工合成麝香酮方面的应用

人工合成已经成为麝香酮的主要来源,但由于原料供应和原料价格问题,许多合成途径都无法实现工业化生产。微生物法生产的长碳链二元酸为人工合成麝香提供了丰富廉价的原料资源,本文概述了以12-16碳二元酸为原料的麝香酮合成途径。     

酮麝香合成过程中硝化反应的研究

从酮麝香合成过程中硝化反应机理入手，选用硫酸作脱水剂，考察了影响产品收率的相关因素，提出了较佳合成工艺条件。