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.     

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 …     

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。     

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。     

合成硝基麝香溶液结晶分离研究

为了开发低共熔组成酮麝香、二甲苯麝香混合物溶液结晶新过程,计算得到酮麝香、二甲苯麝香、溶剂三元相图。在此基础上研究了麝香混合物溶液结晶分离方法,提出了轮流加入乙腈和庚烷从低共熔组成麝香混合物中,分级冷却结晶分离得到2种产品的过程。由三元相图得到理论产量并进行试验验证,结果表明加入乙腈一级结晶可得到纯度为97.5%的二甲苯麝香,加入庚烷二级结晶后酮麝香的纯度为98.1%。     

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。     

双液相萃取棉籽油制备脂肪酸甲酯

以双液相萃取技术处理棉籽,在得到脱毒棉粕的同时得到含有高质量毛油的非极性相。以非极性相作为与甲醇进行酯交换反应的原料,得到脂肪酸甲酯和甘油。考察了非极性相溶剂石油醚与棉籽油的比例对酯交换转化率和洗涤粗产品用水量的影响,确定了石油醚与棉籽油的最佳质量比为3,在此条件下,洗涤用水量可降低一半。考察了醇油比、催化剂用量、反应温度、反应时间等参数对转化率的影响。应用正交实验的方法找出酯交换反应的适宜条件为：醇油比6：1,催化剂用量1.1％,反应温度60℃,反应时间120min。在此反应条件下,产物中脂肪酸甲酯的含量可达97.4％。     

溶液结晶用于分离人造麝香的研究

对酮麝香溶液结晶的分离进行了系统地研究, 给出了全部计算公式, 同时克服了传统结晶器的缺点, 设计了一种可以实现多级分离的结晶器, 并建立了该结晶器的实验装置, 它集结晶、过滤、洗涤于一体。实验结果与计算结果对比令人满意     

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。     

萃取精馏溶剂选择性的温度效应

Extractive distillation is an important and useful technique for separating close boiling and azeotropic liquid mixtures. Solvent selectivity is the key to achieving success. In this paper, the relation of solvent selectivity uersus temperature for different mixed systems (C6H6 C6H12 DMSO,C6H6 C6H12 DMF, EtOH EA DMF DMSO, C6H6 C6 H12 DMF DMSO) was examined by the modified UNIFAC model, which is a well-tested method to select a solvent for extractive distillation.With increasing temperature, solvent selectivity was decreased. In addition, the influence of temperature on solvent selectivity was set forth for the first time by using the Clausius-Mosotti equation.     

动态法筛选萃取精馏分离乙酸丁酯-丁醇-水共沸物的溶剂

采用基于改进UNIFAC模型的动态法对萃取精馏法分离乙酸丁酯-丁醇-水共沸物的萃取剂进行了计算机高通量筛选,根据适宜萃取剂选取原则和计算结果,经综合考虑选出较好的萃取剂为甲醇、乙醇、环氧乙烷。选取乙醇进行实验验证,测定了乙酸丁酯-丁醇-水-乙醇体系的部分汽液平衡实验数据;泡点温度tb、加入溶剂后平衡汽相组成的计算值与实验值吻合良好;以乙醇作为萃取剂具有热负荷小、毒性低和热稳定性好的优点。结果表明,采用基于改进UNIFAC模型的动态法筛选萃取精馏法的溶剂具有良好的可靠性和适用性,可以极大地节省人力、物力和财力。     

减压精馏-熔融结晶耦合装置提纯人造麝香的研究

通过减压精馏-熔融结晶耦合技术研究提高人造麝香(DDHI)含量的原理和工艺流程。实验结果表明,该技术可使人造麝香DDHI的纯度达到98%,总收率达到54%,比原工艺提高13%。     

萃取精馏分离丙醇-水-乙酸丙酯混合物

为挑选萃取精馏分离丙醇-水-乙酸丙酯混合物较好的溶剂,采用基于UNIFAC模型的动态法对待选溶剂进行了计算机高通量筛选。根据加入溶剂后体系互溶性和相对挥发度大小的预测结果,经综合考虑选出较好的萃取剂为丁醇和甲醇。选取丁醇为溶剂做实验验证,测定了丙醇-水-乙酸丙酯-丁醇体系的部分汽液平衡实验数据;泡点温度tb、加入溶剂后的相对挥发度α和平衡气相组成yi的计算值与实验值吻合良好,这表明采用基于UNIFAC模型的动态法筛选萃取精馏的溶剂具有良好的可靠性和适用性。     

气相色谱-质谱联用法测定膏霜类化妆品中10种合成麝香

建立了膏霜类化妆品中10种合成麝香的气相色谱-质谱联用(GC-MS)分析方法。样品加入氘代同位素内标后,用正己烷提取,提取液经基体分散固相萃取(MSPD)净化处理,以VF-WAXms毛细管色谱柱分离,选择特征离子监测(SIM)扫描模式测定,采用标准曲线法定量。结果表明,10种合成麝香的线性范围为0.01~0.2 mg/L,相关系数均大于0.99,定量限为0.05~0.10 mg/kg,加标回收率为80.1%~102.2%,相对标准偏差(RSD)均小于5%。     

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     

Computer‐aided design of ionic liquids as solvents for extractive desulfurization

Although ionic liquids (ILs) have been widely explored as solvents for extractive desulfurization (EDS) of fuel oils, systematic studying of the optimal design of ILs for this process is still scarce. The UNIFAC‐IL model is extended first to describe the EDS system based on exhaustive experimental data. Then, based on the obtained UNIFAC‐IL model and group contribution models for predicting the melting point and viscosity of ILs, a mixed‐integer nonlinear programming (MINLP) problem is formulated for the purpose of computer‐aided ionic liquid design (CAILD). The MINLP problem is solved to optimize the liquid‐liquid extraction performance of ILs in a given multicomponent model EDS system, under consideration of constraints regarding the IL structure, thermodynamic and physical properties. The top five IL candidates preidentified from CAILD are further evaluated by means of process simulation using ASPEN Plus. Thereby, [C₅MPy][C(CN)₃] is identified as the most suitable solvent for EDS. © 2017 American Institute of Chemical Engineers AIChE J, 64: 1013–1025, 2018     

Process intensification on the separation of benzene and thiophene by extractive distillation

The separation of benzene and trace thiophene by extractive distillation was intensified in two aspects, that is, selection of a suitable entrainer and improvement of the process. The mixture of dimethylformamide (DMF) and an ionic liquid (IL) was chosen as the entrainer. Vapor–liquid equilibrium (VLE) experiments using pure DMF and a mixed entrainer were conducted, and UNIFAC model for ILs was extended to the benzene‐thiophene‐DMF‐IL system. The results demonstrated that volatilization loss of DMF in the vapor phase was significantly reduced by adding IL. Moreover, an improved process with only four columns using a mixed entrainer was proposed. The results indicated that the improved process is more promising for decreasing energy consumption and equipment investment compared with the conventional six‐column process. The total heat duties of reboilers and condensers was decreased by 6.47% and 6.41%, respectively. The process intensification strategy may be directly extended to separate trace components of other systems. © 2015 American Institute of Chemical Engineers AIChE J, 61: 4470–4480, 2015