TNAZ溶解度的测定与关联

采用动态法激光检测技术测定了温度为293.15～323.15 K时TNAZ在氯仿、乙醇、乙腈三种溶剂中的溶解度。实验数据采用关联温度和溶解度的apellbat模型[1]、理想溶液模型[2]、多项式经验方程对溶解度数据进行了关联,结果表明上述回归方程均能很好的关联溶解度数据,所得结果可用于工程设计及应用。     

阿奇霉素二水合物在水-有机溶剂中溶解度及三元相图测定

采用静态法测定了293.15～323.15 K范围内，阿奇霉素二水合物在丙酮-水和异丙醇-水混合溶剂中的溶解度，并研究阿奇霉素在293.15、298.15、303.15及308.15 K温度下丙酮-水混合溶剂中转晶水活度，根据溶解度特性绘制丙酮-阿奇霉素-水三元相图，溶解度数据用Apelblat方程、λh方程和van’t Hoff方程进行关联。结果表明，阿奇霉素溶解度随着有机溶剂体积分数和温度的升高而增加，转晶水活度随温度的升高增大，阿奇霉素一水二水共存区域随温度的升高减小，Apelblat方程拟合效果更好，R²≥0.988。     

反式-4-羟基环己基地氯雷他定溶解度测定关联

采用高效液相色谱法测定了常压下在293.15~323.15 K温度范围内反式-4-羟基环己基地氯雷他定在水、质量分数为10% 的甲醇-水、质量分数为20% 的甲醇-水、质量分数为10% 的乙醇-水和质量分数为20% 的乙醇-水中的溶解度,并采用Apelblat方程和λh方程对所得到的溶解度数据进行关联拟合,通过van't Hoff方程计算了其在不同溶剂中的溶解焓和溶解熵。发现反式-4-羟基环己基地氯雷他定的溶解度随着温度的升高和溶剂极性的降低而升高,其溶解过程在实验温度范围内,在所选溶剂中均为吸热熵增过程。     

阿奇霉素二水合物在水-有机溶剂中溶解度及三元相图测定

采用静态法测定了293.15～323.15 K范围内,阿奇霉素二水合物在丙酮-水和异丙醇-水混合溶剂中的溶解度,并研究阿奇霉素在293.15、298.15、303.15及308.15 K温度下丙酮-水混合溶剂中转晶水活度,根据溶解度特性绘制丙酮-阿奇霉素-水三元相图,溶解度数据用Apelblat方程、λh方程和van’t Hoff方程进行关联。结果表明,阿奇霉素溶解度随着有机溶剂体积分数和温度的升高而增加,转晶水活度随温度的升高增大,阿奇霉素一水二水共存区域随温度的升高减小,Apelblat方程拟合效果更好,R~2≥0.988。关键词:阿奇霉素二水合物;溶解度;转晶水活度;Apelblat方程;三元相图     

双季戊四醇在3种混合溶剂中的固-液相平衡

采用动态平衡法,在293.15～332.80 K、常压下,测定了双季戊四醇(DPE)在水+(甲醇、乙醇、异丙醇)三种混合溶剂中的溶解度数据。结果表明：DPE在不同质量分数的水+(甲醇、乙醇、异丙醇)混合溶剂中的溶解度随体系温度升高而增大;同一温度下,其在所选取溶剂体系中的溶解度随着甲醇、乙醇或异丙醇质量分数的增大而先增大后减小。λh方程、两参数方程与Apelblat方程均能够对所测定的溶解度数据进行较好的关联;通过修正的van’t Hoff方程计算得到DPE在所选取溶剂体系中Δ_sol H ⁰、Δ_sol S ⁰和Δ_sol G ⁰均大于零,表明DPE在所选取溶剂体系中的溶解过程为吸热、熵增的非自发过程。     

剑麻皂甙元在甲醇和乙醇中溶解度的测定及应用

常压下,平衡法测定了剑麻皂甙元在甲醇(293~338K)和乙醇(293~353K)溶剂中的溶解度,并对溶解度数据进行关联拟合。结果表明:剑麻皂甙元在两种溶剂中的溶解度均随温度的升高而增大。温度293~323K时,甲醇溶解度高于乙醇溶解度,温度大于323K时,乙醇溶解度高于甲醇溶解度。甲醇和乙醇拟合方程校正决定系数分别为0.9961和0.9976,温度318~338K时,甲醇平均相对误差2.12%,温度328~353K时,乙醇平均相对误差2.56%,拟合方程基本可满足工程设计需要。对两种溶剂在剑麻皂甙元工业生产中的应用进行了研究,表明乙醇作为剑麻皂甙元的萃取溶剂优于甲醇。     

喹诺酮类药物水溶解度的测定与关联

采用平衡法测定了293.15～323.15 K温度范围内6种喹诺酮类药物的水溶解度数据,并运用λh方程进行了关联,确定了方程参数,6种药物的计算与实验值平均相对偏差最大为10.1%.结果表明,实验范围内6种喹诺酮类药物的水溶解度均较小,且分别随温度的升高而略有增加.     

2-丁酮-水-甲苯、环己酮、4-甲基-2-戊酮三元体系液液平衡的测定及关联

测定了2-丁酮-甲苯-水体系在303.15和323.15K、2一丁酮一4一甲基一2一戊酮一水体系在293.15、303.15和313.15K,2-丁酮-环己酮-水体系在293.15和313.15K下的LLE数据.实验数据用NRTL方程关联,部分互溶对和互溶对的方程参数分别从二元和三元LLE数据得到,关联结果与实验数据符合良好.     

甘氨酸在甲醇-水体系中溶解度的测定及关联

本实验采用平衡法测定了293.15—353.15 K下甘氨酸在水中的溶解度,及在不同比例甲醇水溶液中293.15 K至溶液沸点甘氨酸的溶解度。实验结果表明,甘氨酸的溶解度随甲醇摩尔分数的增加而下降,随温度的升高而逐渐增大。分别采用Apelblat方程,λh方程和(CNIBS)/Redlich-Kister方程对溶解度数据进行关联,结果表明:Apelblat方程和λh方程均能较好地表达甘氨酸在甲醇-水体系中的溶解度。(CNIBS)/Redlich-Kister方程能准确地关联溶剂中甲醇的摩尔分数x_2与甘氨酸溶解度x1的关系。利用van't Hoff方程估算得到甘氨酸在甲醇-水中的溶解熵和溶解焓,说明甘氨酸在甲醇-水体系中的溶解过程是吸热和熵驱动的。实验得到的溶解度数据和关联为其工业结晶过程设计和工艺优化提供了理论依据。     

六水氯化镁在醇类溶剂中溶解度的测定与关联

使用平衡法测定了在293.15~338.15 K时,六水氯化镁在乙醇、正丙醇、异丙醇、丙三醇、正丁醇、异丁醇六种醇类有机溶剂中的溶解度。实验结果表明六水氯化镁在六种醇类有机溶剂中的溶解度均随着温度的升高而增大,且在丙三醇、乙醇中的溶解度相对较大。采用Apelblat方程、λh方程、理想状态方程和多项式经验方程分别对溶解度实验数据进行关联,关联结果良好,其中Apelblat方程拟合结果优于其他三种方程。所得实验数据和拟合模型为六水氯化镁在非水体系中的应用提供了重要依据。     

苯基周位酸溶解度的测定及其影响因素的考察

溶解度是结晶工艺研究的基础数据,对结晶工艺的优化,最终收率的预测具有重要的指导作用。采用激光法测定了苯基周位酸在水和乙醇-水混合溶剂的溶解度,并讨论了几个因素对溶解度的影响。     

二苯基亚砜在有机溶剂中的溶解度测定和拟合

在温度288.30～334.32 K、常压条件下,采用合成法测定二苯基亚砜在乙醇、乙酸乙酯、甲苯、丙酮、氯仿以及一系列浓度的乙醇-水混合溶剂中的溶解度。实验结果表明,在相同温度下,5种纯溶剂中二苯基亚砜的溶解度大小顺序如下,氯仿 > 丙酮 > 甲苯 > 乙酸乙酯 > 乙醇;乙醇-水混合溶剂中溶解度随着乙醇浓度下降而迅速降低;该溶解过程为吸热熵增过程,且随着溶解Gibbs斯自由能增大,溶解度减小。数据采用改进的Apelblat方程和van’t Hoff方程进行拟合,在乙醇-水混合溶剂中的溶解度数据还采用Jouban-Acree方程拟合。拟合结果与实验数据基本吻合。测定的固液平衡数据可为二苯基亚砜的合成与提纯等过程的溶剂选择提供依据。     

对苯二甲酸和对羧基苯甲醛在醋酸水溶液中的溶解度

测定了420-505K温度范围内,对苯二甲酸和对羧基苯甲醛在醋酸水溶液中溶解度。在70%-100%醋酸水溶液中,70%醋酸使对苯二甲酸的溶解度对温度最敏感,随着醋酸浓度增加,对苯二甲酸的溶解度减少。当温度低于470K时,对苯二甲酸在水中的溶解性低于醋酸中的溶解度;温度高于470K时,对苯二甲酸在水中的溶解性对温度敏感明显提高。40%醋酸使对羧基苯甲醛的溶解度对温度最敏感, 随着醋酸浓度增加, 对羧基苯甲醛的溶解度增加。实验数据用修正的Apelblat方程进行了对苯二甲酸和对羧基苯甲醛在醋酸水溶液中溶解度关联,计算与实验值吻合良好。     

Determination and correlation solubility of m-phenylenediamine in (methanol,ethanol, acetonitrile and water) and their binary solvents from 278.15 K to 313.15 K

In this study, the solubility of m-phenylenediamine in four pure solvents(methanol, ethanol, acetonitrile and water) and three binary solvent(methanol + water),(ethanol + water) and(acetonitrile + water) systems were determined in the temperature ranging from 278.15 K to 313.15 K by using the gravimetric method under atmospheric pressure. In the temperature range of 278.15 K to 313.15 K, the mole fraction solubility values of m-phenylenediamine in water, methanol, ethanol, and acetonitrile are 0.0093–0.1533, 0.1668–0.5589,0.1072–0.5356, and 0.1717–0.6438, respectively. At constant temperature and solvent composition, the mole fraction solubility of o-phenylenediamine in four pure solvents was increased as the following order:water b ethanol b methanol b acetonitrile; and in the three binary solvent mixtures could be ranked as follows:(ethanol + water) b(methanol + water) b(acetonitrile + water). The relationship between the experimental temperature and the solubility of m-phenylenediamine was revealed as follows: the solubility of mphenylenediamine in pure and binary solvents could be increased with the increase of temperature. The experimental values were correlated with the Jouyban–Acree model, van't Hoff–Jouyban–Acree model, modified Apelblat–Jouyban–Acree model, Sun model and Ma model. The standard dissolution enthalpy, standard dissolution entropy and the Gibbs energy were calculated based on the experimental solubility data. In the binary solvent mixtures, the dissolution of m-phenylenediamine could be an endothermic process. The solubility data,correlation equations and thermodynamic property obtained from this study would be invoked as basic data and models regarding the purification and crystallization process of m-phenylenediamine.     

Thermodynamic properties of metamizol monohydrate in pure and binary solvents at temperatures from (283.15 to 313.15)K

The thermodynamic properties of metamizol monohydrate in pure solvents (methanol,ethanol,n-propanol and isopropanol) and two binary mixed solvent systems including (methanol + ethanol) and (methanol +isopropanol) were measured from 283.15 K to 313.15 K by gravimetric method under atmospheric pressure thought as 0.1 MPa.The modified Apelblat equation,the CNIBS/R-K equation,the Hybrid model and the NRTL model were used to correlate the solubility of metamizol monohydrate,respectively.The results show that the solubility of metamizol monohydrate in all the tested solvents increases with the rising temperature which means that it has temperature dependence.What's more,the effects of solvent components of the binary solvent mixtures on solubility were discussed,it illustrates that the increasing of the molar fraction of methanol gives the system a greater dissolving power.Furthermore,according to the NRTL model,the enthalpy,the Gibbs energy and the entropy of the mixing process were also obtained and discussed.     

Measurement and correlation of solubility of meropenem trihydrate in binary (water + acetone/tetrahydrofuran) solvent mixtures

The solubility of meropenem trihydrate in water + acetone mixtures and water + tetrahydrofuran mixtures were determined from T =(278.15 to 303.15) K by static method under atmospheric pressure.Effects of solvent composition and temperature on solubility of meropenem trihydrate were discussed.To extend the applicability of the solubility data,experimental solubility data in two kinds of binary solvent mixtures were correlated by the Apelblat equation and NIBS/Redlich-Kister model.It was found that the two models could satisfactorily correlate the experimental data and the Apelblat equation could give better correlation results.     

Solubilities of Isophthalic Acid in Acetic Acid + Water Solvent Mixtures

The solubilities of isophthalic acid (1) in binary acetic acid (2)+water (3) solvent mixtures were determined in a pressurized vessel. The temperature range was from 373.2 to 473.2K and the range of the mole fraction of acetic acid in the solvent mixtures was from x₂ 0 to 1. A new method to measure the solubility was developed, which solved the problem of sampling at high temperature. The experimental results indicated that within the temperature range studied, the solubilities of isophthalic acid in all mixtures showed an increasing trend with increasing temperature. The experimental solubilities were correlated by the Buchowski equation, and the calculate results showed good agreement with the experimental solubilities. Furthermore, the mixed solvent systems were found to exhibit a maximum solubility effect on the solubility, which may be attributed to the intermolecular association between the solute and the solvent mixture. The maximum solubility effect was well modeled by the modified Wilson equation.     

十二烷基苯磺酸钠-乙醇-水体系固液相平衡

引　言烷基苯磺酸盐是目前已发现的高效廉价驱油用表面活性剂[1,2 ] ,在用于三元 (表面活性剂、碱和聚合物 )复合驱技术时[1,2 ] ,体系中常加入醇类助剂 ,以进一步降低油水界面张力和扩大体系的均相区[3,4 ] .在进行驱油体系配方筛选时 ,急需相平衡知识的理论指导 .本文实验测定了 2 98.15～318.15Ｋ十二烷基苯磺酸钠 (ＳＤＢＳ)在乙醇 -水混合溶剂中的溶解度 ,实验结果用溶解度模型关联 .1　实验测定用浊度法测定溶解度 ,实验装置和操作步骤见文献 [5 ],测定时控温精度为± 0 .1Ｋ .样品为 :①ＳＤＢＳ ,分析纯 ;②无水乙醇 ,分析纯 ;③氢…     

紫杉醇在二氯甲烷-超临界二氧化碳混合溶剂中的溶解度

Phase behavior of paclitaxel in solvent mixtures of dichloromethane and supercritical carbon dioxide was investigated using a supercritical phase monitor. Cloud point pressures were determined as a function of temperature, pressure and paclitaxel content from 313.1 to 343.1 K and pressures up to 33.52 MPa. The ternary mixtures exhibit a typical lower critical solution temperature behavior. When paclitaxel content increases, the single-phase region shrinks in size. Three cubic equations of state (Redlich-Kworng, Soave-Redlich-Kwong and Peng-Robinson equation of state) coupled with the van der Waals one-fluid mixing rules were selected to correlate the experimental data. The results indicate that SRK EOS coupled with two binary interaction parameters kij and lij can pre-dict paclitaxel solubility for the best fit of experimental data.     

Solubility of D(−)-p-hydroxyphenylglycine dane salt in binary methanol+isopropanol solvent mixtures

The solubility of D(−)-p-Hydroxyphenylglycine Dane Salt (HPGDane Salt) in binary methanol and isopropanol solvent mixtures was measured using a laser technique with the temperature range from 283.15 K to 323.15 K and mole fraction (x₂) range from 0.0000 to 1.0000. The results were correlated with a semi-empirical equation.