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CHINESE JOURNAL OF CHEMICAL ENGINEERING · 2022 · IF 3.898

Design and optimization of purification process of sinomenine hydrochloride

Dandan Ren,Shanshan Xiang,Yuwen Yan,Ruiying Kong,Xingchu Gong

Sinomenine hydrochloride is generally produced from Caulis Sinomenii . At present, the purification process in industrial production suffers from large amount of solid waste, high solvent toxicity, and low sinomenine hydrochloride yield. In this study, a new purification process for sinomenine hydrochloride was proposed by using the extract obtained from acid extraction of Caulis Sinomenii as the starting material. The process included the following steps: alkalization, extraction, water washing, acid–water stripping, drying, and crystallization. 1-Heptanol was used as the extractant. The distribution coefficients of sinomenine and sinomenine hydrochloride in 1-heptanol–water system were 27.4 and 0.0167, respectively. The dissociation constants of sinomenine hydrochloride were 8.27 and 11.24, respectively. Process parameters of the new purification process were optimized with experimental design. The extractant 1-heptanol and sinomenine hydrochloride in the crystallization mother solution can be recycled in the new process. The purity of the obtained sinomenine hydrochloride crystals exceeded 85%, and the yield was about 70%. Compared with current industrial processes, safer extractant, less solid waste, and higher sinomenine hydrochloride yield can be achieved using the new purification process of sinomenine hydrochloride provided in this study.

CAS / MDL: 107-15-3
研究领域: 中药化学 · 制药工程
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JOURNAL OF CHEMICAL AND ENGINEERING DATA · 2023 · IF 2.6

Liquid–Liquid Equilibrium Measurement and Thermodynamic Modeling for Ternary Systems of 1,3-Propanediol + 2-Propyl-1-heptanol + Extractants at 298.2 K

Jiajun Wei,Lingxiao Yi,Wang Yuxin,Erkang Li,Zhen Yujie,Fangyu Zhang,Xinlei Niu,Jinshan Wang,Deming Zhao,Yingmin Yu

Liquid–liquid equilibrium (LLE) measurements were conducted at a temperature of 298.2 K and a pressure of 101.3 kPa for the ternary system consisting of 1,3-propanediol, 2-propyl-1-heptanol, and various extractants (n-hexane, vinyl acetate, ethyl benzene, and water). By calculating the distribution constant (D) and selectivity (S) in each system, the ability of four extractants to separate the mixture of 1,3-propanediol and 2-propyl-1-heptanol was compared. Furthermore, the LLE data underwent regression using thermodynamic models NRTL and UNIQUAC. The degree of deviation between the experimental data and regression data was assessed using the root mean square deviation (RMSD) and the average absolute deviation (AAD). The RMSD values for the NRTL and UNIQUAC models were below 0.74 and 0.76%, respectively, with corresponding AAD values below 0.39 and 0.60%. These results indicate a robust concurrence between the experimental data and the outcomes of the regression analysis. Finally, the GUI-MATLAB tool was employed to validate the coherence of the experimental data with the regression parameters. σ-Profiles are used to discuss the interactions of substances in this work. The results showed that the D and S of all four systems were greater than 1, indicating that all four extractants were effective in separating 1,3-propanediol and 2-propyl-1-heptanol. The order of their extraction capacity was water ≥ hexane ≥ ethyl benzene ≥ vinyl acetate.

研究领域: 化学工程 · 热力学
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JOURNAL OF CHEMICAL THERMODYNAMICS · 2022 · IF 3.269

Liquid-liquid equilibrium data for ternary mixtures (water + isopropanol + 1-pentanol/1-hexanol/1-heptanol) at 298.15 K: Measurement, correlation and prediction

Wenyang Fan,Yuanyuan Han,Houchun Yan,Dongmei Xu,Huiwen Huang,Yinglong Wang

To recover isopropanol from its aqueous solution, alkanols (1-pentanol, 1-hexanol and 1-heptanol) were selected as the solvents to separate water and isopropanol. Liquid-liquid equilibrium data for water + isopropanol + 1-pentanol/1-hexanol/1-heptanol ternary systems were measured at 298.15 K under 101.3 kPa. The mass conservation of the experimental data was checked, and the reliability of the tie-lie data were evaluated by the Bachman, Hand and Othmer-Tobias equations. The extraction performance of the three solvents was assessed through the separation factor and partition coefficient, and compared with those for other reported solvents {esters, ketones, ethers, alkanes (or alkenes), ionic liquids and deep eutectic solvents}, indicating that 1-heptanol has better extraction performance for isopropanol compared with other two solvents. The NRTL and UNIQUAC models were used to correlate the data to obtain regression parameters. The mixed surface analysis based on Gibbs energy topology verified that the binary interaction parameters are consistent with the measured data. Furthermore, the LLE binodal curve for the researched ternary systems were predicted through the UNIFAC and COSMO-UNIFAC models.

研究领域: 化学工程 · 物理化学 · 热力学
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JOURNAL OF CHEMICAL AND ENGINEERING DATA · 2025 · IF 2.1

Liquid-Liquid Equilibrium Measurement and Modeling of Methyl 2-Hydroxyisobutyrate, Water, and Different Extractants at 303.2 K

He Ma,Houchun Yan,Menghao Du,Yingmin Yu,Qingsong Li

To separate methyl 2-hydroxyisobutyrate from an aqueous solution, alkyl alcohols were selected as extractants. The liquid–liquid equilibrium data for the system {water + methyl 2-hydroxyisobutyrate + extractants (1-hexanol, 1-heptanol, 1-octanol, and 1-nonanol)} were determined at a temperature of 303.2 K. The partition coefficients and separation factors were calculated to assess the effectiveness of the extraction process. Additionally, the data were correlated using the NRTL and UNIQUAC models, with parameter regression conducted accordingly. The GMcal_TieLinesLL tool was utilized to evaluate the regression model parameters, and the results conformed to the Gibbs stability criterion. The present study further investigates the separation mechanism through analyses of σ-profile, deformation charge density, interaction energies, and Reduced Density Gradient (RDG) analysis. Ultimately, it was concluded that 1-nonanol exhibited the most effective extraction performance.

研究领域: 化学工程 · 分离过程 · 物理化学 · 热力学 · 萃取 · 分子建模
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