合成硝基麝香在溶剂中固液平衡研究

采用综合法测定了合成硝基麝香在乙腈等溶剂中的固液平衡数据,采用UNIFAC方程对麝香在单一溶剂中的固液平衡数据进行了关联,结果表明UNIFAC方程能够较好地关联实验数据并具有一定的预测功能,为麝香混合物的溶液结晶分离提供了理论依据。     

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。     

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。     

UNIFAC基团贡献法预测合成硝基麝香固液平衡

UNIFAC基团贡献法是目前流行的一种重要的推算相平衡的方法.应用UNIFAC基团贡献法研究了合成硝基麝香物系在乙酸乙酯、乙睛、环已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,误差在允许的范围之内,能满足合成硝基麝香体系固液平衡计算的需要.     

合成硝基麝香三元体系的固液平衡

通过试验测定了合成硝基麝香二元体系的固液平衡数据,回归并修正了UNIFAC模型的相互作用参数,使UNIFAC模型具有更高的预测功能;为了评价修正后的UNIFAC模型对合成硝基麝香三元体系的预测功能,利用试验测定的溶解度数据和修正后的UNIFAC模型计算值进行了比较,结果表明相互作用参数的修正是理想的.     

酮麝香与二甲苯麝香体系相平衡研究

为了判断酮麝香、二甲苯麝香固相存在状态,改进Lennard-Jonnes位能函数后得到了适用于极性和非极性分子的位能函数式,计算得到酮麝香、二甲苯麝香体系相互作用能量参数λ,结合NRTL方程计算确认酮麝香、二甲苯麝香为简单低共熔体系,采用差分扫描量热热分析法进行了实验验证。     

三元体系LiBr-Li2SO4-H2O 298 K相平衡

为了获取地下卤水中的锂盐的溶解和析盐规律,进一步指导开发宝贵的液态锂资源,文中采用等温溶解平衡法研究了三元体系LiBr-Li_2SO_4-H_2O在298 K时的固液稳定相平衡关系,测定了平衡溶液的饱和溶解度和密度,并根据饱和液相组成、湿固相组成和对应的平衡固相绘制了等温溶解度图和密度-组成图。结果表明:三元体系在298 K时的相图为简单共饱和型相图,平衡固相中无复盐和固溶体形成;该体系的相图由一个共饱点E,2条单变量溶解度曲线AE和BE,2个单盐结晶区组成,其中结晶区分别对应于二水溴化锂和一水硫酸锂;在三元体系中,溴化锂对硫酸锂有明显的盐析作用,且一水硫酸锂的结晶区远大于二水溴化锂。平衡液相对应的饱和固相由湿渣法和XRD确定。     

邻苯二甲酸酐和顺丁烯二酸酐在水中的溶解度研究

本文研究了萘气相催化氧化制备1,4-萘醌的工业副产物的分离,其副产物主要是邻苯二甲酸酐和顺丁烯二酸酐,对其加以提纯和分离,将可以重新利用。溶质溶解结晶法是固体实现混合物中各成分分离的有效方法,但需要预先知道固体混合物中各成分在溶剂中的溶解度,然后对固—液体系进行研究。所以本文主要针对邻苯二甲酸酐,顺丁烯二酸酐分别在水中的溶解度进行固-液相平衡的基础研究。通过了动态法测出了邻苯二甲酸酐和顺丁烯二酸酐在水中的溶解度,根据测定的结果可以看出这两种副产物在水中的溶解度数据相差较大,水可以作为最佳的分离溶剂。     

对苯二甲酸在水和醋酸体系中相平衡测定与关联

在一定温度下 ,对苯二甲酸、水和醋酸达到固液平衡 ,体系为饱和溶液 ,利用标准氢氧化钠溶液滴定饱和溶液中溶质的含量来测定对苯二甲酸。同时 ,采用热力学模型关联实验数据 ,结果令人满意。     

戊二酸在环己烷、环己酮、环己醇中溶解度的研究

戊二酸的工业生产方法是从环己烷氧化制取己二酸所得的副产物中回收而得。其中环己烷氧化的中间产物主要有环己酮和环己醇,与戊二酸共存的有丁二酸、己二酸等有机物。对戊二酸在环己烷、环己酮、环己醇中的溶解度进行研究,可为戊二酸分离提纯工艺条件的选择及优化提供基础数据。本文利用常压固液平衡测定装置,采用简便易行的溶解度测定方法,对戊二酸在环己烷、环己酮、环己醇单一溶剂及其混合溶剂中的溶解度进行了测定。结果表明,在20℃时,戊二酸在环己醇中溶解度最大,为30．5316g;在环己烷中的溶解度最小,只有0．0318g。在三种溶剂的混合体系中,随着醇酮含量的增加,戊二酸的溶解度增大;当温度低于30℃时,环己酮和环己醇的混合对戊二酸的溶解存在协同效应。     

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 …     

Method for predicting solubilities of solids in mixed solvents

A method is presented for predicting solubilities of solid solutes in mixed solvents, based on excess Henry's law constants. The basis is statistical mechanical fluctuation solution theory for composition derivatives of solute/solvent infinite dilution activity coefficients. Suitable approximations are made for a single parameter characterizing solute/solvent interactions. Comparisons with available data show that the method is successful in describing a variety of observed mixed solvent solubility behavior, including nearly ideal systems with small excess solubilities, systems with solute‐independent excess solubilities, and systems deviating from these simple rules. Successful predictions for new solvent mixtures can be made using limited data from other mixtures. © 2009 American Institute of Chemical Engineers AIChE J, 2009     

Solubility prediction of bioantioxidants for functional solvent by group contribution method

Bioantioxidants protect a living body from the damage and ageing caused by active oxygen. Typical bioantioxidants include epicatechin, caffeic acid, ascorbic acid, etc. This study focused on selecting the optimum solvent that can dissolve each bioantioxidants by calculating the solubility of various bioantioxidants in each specific solvent. The solubility parameters of the bioantioxidants were correlated with the van Krevelen group model, and the solubility of bioantioxidant for each solvent was then calculated from the interaction relationship between each solubility parameter of the bioantioxidant and optimal solvent selected. The solubility of the bioantioxidants was affected not only by the solubility parameters of the solute and solvents, but also by the fusion enthalpy of the solute at melting temperature. Then the fusion enthalpy was measured for each bioantioxidant. The equilibrium non-ideality between the solvent and bioantioxidants examined as a function of the solubility parameter and fusion enthalpy. The optimum solvent was selected for each bioantioxidant based on the quantitative solubility data. Each bioantioxidant showed slight non-ideality, which it was presented in the activity coefficient of the solution system.     

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。     

Generalizing solubility parameter theory to apply to one‐ and two‐dimensional solutes and to incorporate dipolar interactions

Hildebrand and Hansen solubility parameters are commonly used to identify suitable solvents for the dispersion or dissolution of a range of solutes, from small molecules to graphene. This practice is based on a number of equations, which predict the enthalpy of mixing to be minimized when the solubility parameters of solvent and solute match. However, such equations have only been rigorously derived for mixtures of small molecules, which interact only via dispersive forces. Herein, we derive a general expression for the enthalpy of mixing in terms of the dimensionality of the solute, where small molecules are considered zero‐dimensional, materials such as polymers or nanotubes are one‐dimensional (1D) and platelets such as graphene are two‐dimensional (2D). We explicitly include contributions due to dispersive, dipole–dipole, and dipole‐induced dipole interactions. We find equations very similar to those of Hildebrand and Hansen so long as the solubility parameters of the solute are defined in a manner which reflects their dimensionality. In addition, the equations for 1D and 2D systems are equivalent to known expressions for the enthalpy of mixing of rods and platelets, respectively, as a function of surface energy. This agreement between our expressions and those commonly used shows that the concept of solubility parameters can be rigorously applied to extended solutes such as polymers, nanotubes, and graphene. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Solubility of 1-monostearin in various solvents

Summary The practical limits of the solubility of pure monostearin in various solvents at different temperatures has been determined for isopropyl alcohol, ethanol, acetone, methanol, and commercial hexane. The synthetic method was employed, in which the temperature of known quantities of solvent and solute was decreased until crystallization of the solute began. This temperature, corrected for supercooling and heat loss to the surrounding bath, was taken as the equilibrium temperature between the known weight of solute and the known weight of solvent. The solubility-temperature data of monostearin in each of the various solvents are presented both graphically and in tabular form. A comparison of the solubility of monostearin in the various solvents at comparative temperatures indicates that its solubility is greatest in isopropyl alcohol and decreases in the order ethanol, acetone, methanol, and hexane. Presented at the 45th annual meeting of the American Oil Chemists' Society, San Antonio, Tex., April 12–14, 1954. One of the laboratories of the Southern Utilization Research Branch, Agricultural Research Service, U. S. Department of Agriculture.     

Solvent extraction using dialysis through artificial phase boundaries

Several solvent extraction systems were studied using a cellulose dialysis membrane as an artificial phase boundary separating one solvent phase from the other. Solutes were allowed to come to extraction equilibrium by permeation through the membrane. The rate of permeation depended on the osmotic properties of the solute, such as the molecular size and the presence of colloidal species. The extraction equilibrium was established by the solvent-extraction properties of the solute in each system, and the equilibrium was approached through the cellulose membrane by a first-order kinetic process. The method appears to be useful for ‘packaging’ organic solvents in membrane containers to be used for extractions in which time is not a factor. In certain cases, equally well extracted solutes, such as zirconium and aluminium 8-hydroxyquinolates, can be separated because one solute exists as a partially colloidal material [Zr(IV)] and hence does not pass through the membrane rapidly.     

Solubilities of anthracene,fluoranthene and pyrene in organic solvents: Comparison of calculated values using UNIFAC and modified UNIFAC (Dortmund) models with experimental data and values using the mobile order theory

The solubility of anthracene in 43 organic solvents, fluoranthene (45 solvents) and pyrene (30 solvents) has been calculated using UNIFAC and Modified UNIFAC (Dortmund) models to estimate the activity coefficient of the solute. It was found that both UNIFAC and Modified UNIFAC described better the solubilities in polar solvents like alcohols, ketones, esters and ethers than in nonpolar solvents like alkanes and aromatic hydrocarbons. UNIFAC and the Mobile Order Theory supplement each other well in calculating the solubilities, which means that one can choose the right model depending on the solvent one is using.     

人造麝香DDHI重结晶的研究

测定了人造麝香DDHI在不同质量分数的乙醇水溶液中的溶解度 ,并用重结晶的方法提纯DDHI,适宜的工艺条件为 :用质量分数为 80 %的乙醇水溶液作为溶剂 ,将液态DDHI溶于 6 0℃的溶剂中 ,缓慢冷却至 2 0℃进行重结晶 ,溶液的pH =7,乙醇水溶液与DDHI的质量比为 2 3～2 6 ,进行二至三次重结晶可得到质量分数大于 99 5 %的DDHI     

计算机辅助筛选分离联苯与4-联苯乙酮两种化合物的溶剂

引言 4-联苯乙酮是合成非甾体抗炎药联苯乙酸和液晶材料的重要精细化工中间体[1].以联苯为原料,在无水三氯化铝存在下,用乙酰氯或醋酐进行傅一克反应可合成4-联苯乙酮[2-3];反应结束后加入碎冰和盐酸水解,然后静置分层,分出油层,水层用二氯乙烷多次萃取;萃取物并入油层,减压蒸去溶剂后可得到4-联苯乙酮粗品;文献[4]以氯仿为萃取剂从水层中提取目的产物.