本文選題：手性分離 + 多級離心萃取��； 參考：《湖南理工學(xué)院》2017年碩士論文

【摘要】：本論文以親水性β-環(huán)糊精衍生物為手性萃取劑,對藥物中間體(2-苯基丁酸、托品酸與2,3-二苯基丙酸對映體)的多級離心萃取分離過程進行了研究。聯(lián)立液-液萃取理論模型與質(zhì)量守恒定律,結(jié)合相平衡方程,分別建立了相應(yīng)的離心萃取的數(shù)學(xué)模型,運用Matlab軟件編寫程序,建立的模型用于模擬和優(yōu)化多級離心萃取分離過程,得到了一系列的離心萃取分離過程的規(guī)律以及工藝操作參數(shù),為分離這3種藥物中間體以及離心萃取器的設(shè)計和放大提供了科學(xué)依據(jù)。本論文的主要研究工作和結(jié)果如下:1.液-液萃取實驗,分別考察了有機溶劑、環(huán)糊精種類、溫度、水相pH等因素對分配比(D)和分離因子(α)的影響。得到了相應(yīng)的最佳萃取條件。在278 K下,以1,2-二氯乙烷為有機溶劑,羥乙基-β-環(huán)糊精(HE-β-CD)為手性萃取劑,水相pH為3.0,萃取2-苯基丁酸的分離因子最佳為2.096。以乙酸丁酯為有機溶劑、羥乙基-β-環(huán)糊精(HE-β-CD)為手性萃取劑、水相pH為3.0,萃取托品酸的分離因子最佳為1.606。以1,2-二氯乙烷為有機溶劑、璜丁基-β-環(huán)糊精(SBE-β-CD)為手性萃取劑、水相pH為3.0,萃取2,3-二苯基丙酸的分離因子最佳為1.422。2.聯(lián)立液-液萃取理論與質(zhì)量守恒定律,結(jié)合相平衡方程,建立多級離心萃取過程模型,運用Matlab平臺編寫程序,模擬多級離心萃取過程各因素的影響。通過實驗與模型模擬,考察了離心機轉(zhuǎn)速、兩相流量比(W/O、O/W和W/F)、環(huán)糊精濃度、水相pH值、以及萃取級數(shù)等因素對多級離心萃取性能的影響。結(jié)論如下:在最佳操作條件下,分離2-苯基丁酸對映體,eeeq達到97%與99%以上所需的萃取級數(shù)分別為60級與82級;分離托品酸對映體,eeeq達到97%與99%以上所需的萃取級數(shù)分別為56級與78級;分離2,3-二苯基丙酸,eeeq達到97%與99%以上所需的萃取級數(shù)分別為78級與102級。
[Abstract]:In this paper, using hydrophilic 尾 -cyclodextrin derivatives as chiral extractant, the separation process of 2-phenylbutyric acid, tropinic acid and enantiomers of 2-diphenyl propionic acid was studied. The theoretical model of simultaneous liquid-liquid extraction and the law of conservation of mass, combined with the equation of phase equilibrium, were used to establish the corresponding mathematical model of centrifugal extraction, and the program was written by using Matlab software. The model is used to simulate and optimize the separation process of multistage centrifugal extraction. It provides a scientific basis for the separation of these three drug intermediates and the design and amplification of centrifugal extractors. The main work and results of this thesis are as follows: 1. The effects of organic solvent, type of cyclodextrin, temperature and pH of aqueous phase on the partition ratio (D) and separation factor (偽) were investigated. The optimum extraction conditions were obtained. At 278K, the best separation factor of 2-phenylbutyric acid was 2.096, with 1h2- dichloroethane as organic solvent and hydroxyethyl 尾 -cyclodextrin HE- 尾 -CD) as chiral extractant. The pH of aqueous phase was 3.0, and the separation factor of 2-phenylbutyric acid was 2.096. When butyl acetate was used as organic solvent, hydroxyethyl 尾 -cyclodextrin (HE- 尾 -CD) was used as chiral extractant, pH was 3.0 in aqueous phase, the best separation factor was 1.606. The best separation factor for extraction of 2-diphenylpropionic acid was 1.422.2 with 1 ~ (2 +) -dichloroethane as organic solvent, Juan Ding Ji-尾 -cyclodextrin (SBE- 尾 -CDCD) as chiral extractant, pH = 3.0 in aqueous phase. The simultaneous liquid-liquid extraction theory and mass conservation law combined with phase equilibrium equation were used to establish a multistage centrifugal extraction process model. The program was compiled by using Matlab platform to simulate the influence of various factors in the multistage centrifugal extraction process. The effects of centrifuge speed, two-phase flow ratio (W / O / O / W and W / F), concentration of cyclodextrin, pH value of water phase and extraction order on the performance of multistage centrifugal extraction were investigated by experiments and model simulation. The results are as follows: under the optimum operating conditions, the extraction order required for the separation of 2-phenylbutyric acid enantiomers is 60 and 82, respectively, when the enantiomers are 97% and 99% respectively. The order of extraction required for separation of enantiomeric enantiomers of tropinic acid is 56 and 78, respectively, and the extraction order for separation of enantiomeric enantiomers of tropicanoic acid is 97% and 99%, respectively, and the order of extraction is 78 and 102 for separating the enantiomeric enantiomers of tropicaric acid, which are above 97% and 99%, respectively.
【學(xué)位授予單位】：湖南理工學(xué)院
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：O658.2;TQ460.1

【參考文獻】

相關(guān)期刊論文 前10條

1 左臣;李傳博;晏太紅;鄭衛(wèi)芳;袁中偉;曹智;孫雪梅;;鈾钚萃取洗滌-共反萃工藝的離心萃取器臺架實驗研究[J];原子能科學(xué)技術(shù);2015年06期

2 周叢山;徐萍;唐課文;蔣新宇;楊濤;張盼良;朱政;;Enantioselective extraction of clorprenaline enantiomers with hydrophilic selector of sulfobutylether-β-cyclodextrin by experiment and modeling[J];Journal of Central South University;2014年03期

3 張金彥;吉紹長;;藥物的手性拆分[J];化學(xué)通報;2013年08期

4 鄭燁;顏繼忠;童勝強;李行諾;楚楚;;高效液相色譜手性流動相添加法拆分2-苯丙酸對映體[J];藥物分析雜志;2013年05期

5 徐艷;張保棟;張艷紅;白志山;;環(huán)隙式離心萃取分離技術(shù)研究進展[J];合成纖維工業(yè);2012年04期

6 林祖武;;HPLC法測定苦參洗劑中苦參堿的含量[J];中醫(yī)藥導(dǎo)報;2011年10期

7 李亮洪;李芬芳;邢健敏;;手性藥物拆分新方法研究進展[J];化工技術(shù)與開發(fā);2011年04期

8 張德友;卓培忠;李傳祥;陳道林;陳崔龍;陳建國;;新型離心萃取機的開發(fā)及其應(yīng)用前景[J];過濾與分離;2008年03期

9 ;Resolution of α-cyclohexyl-mandelic acid enantiomers by two-phase (O/W) recognition chiral extraction[J];Science in China(Series B:Chemistry);2007年06期

10 徐剛;程詠梅;吳堅平;楊立榮;;有機相酶催化拆分制備(S)-2-氯-1-(2-噻吩)-乙醇[J];有機化學(xué);2007年07期

相關(guān)碩士學(xué)位論文 前2條

1 王亞瓊;多級離心萃取手性分離藥物外消旋體研究[D];湘潭大學(xué);2015年

2 程永琪;手性液膜技術(shù)用于布洛芬外消旋體拆分過程的研究[D];北京化工大學(xué);2012年

，

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