模拟移动床色谱分离技术综述

本文对模拟移动床的建模、模型求解和优化进行了综述,介绍了几种常用的色谱模型以及模型的求解方法和优化策略。在结构优化方面,本文重点介绍了在模拟移动床基础上改进的间歇模拟移动床色谱分离技术。间歇模拟移动床技术通过改变色谱柱的数量来实现分离过程,和常规的模拟移动床技术相比较,它的设计结构简单、成本低,并且比常规的模拟移动床具有更高的分离性能。     

模拟移动床色谱在手性药物大规模拆分中的应用

模拟移动床色谱作为手性药物大规模拆分领域中的强有力工具,越来越受到人们的重视,该文介绍了模拟移动床色谱技术的发展情况及其工作原理,对描述模拟移动床色谱分离行为的理论模型和分离操作中操作参数的确定也作了介绍。     

模拟移动床色谱技术及其应用

详细地介绍了一种现代化分离技术模拟移动床色谱技术的发展历史及其工作原理,同时介绍了模拟移动床色谱在石油化工、糖醇分离、手性化合物及其他方面的主要应用。     

我国研发的模拟移动床分离色谱技术酝酿新突破

我国自主研发的模拟移动床色谱分离技术继成功用于天然产物活性成分提取后,又在酝酿新的突破。不久前,黑龙江省八一农垦大学与上海石油化工研究院、华东理工大学石油研究所签订了模拟移动床设备研发合作协议书,将研制适合高温高压条件下使用的烃类化工设备,石油化工、生物产业将成为这一精细分离技术的又一个用武之地。模拟移动床色谱分离技术是一种高效、先进的分离纯化技术,应用领域遍及石油化工、食品、精细化工、生物发酵和医药等。     

简讯

<正>我国研发的模拟移动床分离色谱技术酝酿新突破我国自主研发的模拟移动床色谱分离技术继成功用于天然产物活性成分提取后,又在酝酿新的突破。不久前,黑龙江省八一农垦大学与上     

基于浮点编码的遗传算法优化模拟移动床色谱分离木糖醇母液

开发了一种基于浮点编码遗传算法的模拟移动床色谱优化方法。该优化方法中将归一化的生产强度取最大值作为目标函数,同时将纯度的n次方作为罚函数。运算过程中浮点编码遗传算法的适度值由模拟移动床色谱的稳态模型求得。为了保证遗传算法每一代的个体均满足模拟移动床色谱本身的约束条件,算术杂交和完全非均匀变异被用作演化算子。采用该算法很容易得到模拟移动床色谱分离过程中非线性条件下的最优条件。这种优化算法被应用于木糖醇母液的模拟移动床色谱,结果表明当罚函数指数n值由小到大变化时,可以得到产品纯度由低到高的最优分离条件。进一步     

工业制备色谱在中药分离制备中的应用

概述了工业制备色谱柱型结构、填料、色谱技术特性的研究进展,对目前普遍使用的工业制备色谱的工作原理作了较为全面的评述,总结了动态轴向压缩色谱和模拟移动床色谱技术在中药分离制备中的应用和发展。     

模拟移动床色谱法拆分甲霜灵对映体

模拟移动床(SMB)色谱作为一种精确、高效的制备色谱技术引起研究者的极大关注。本文以EnantioPak OD填料为手性固定相,正己烷-乙醇(70 : 30, v/v)为流动相,在四区模拟移动床上手性拆分甲霜灵外消旋体。采用旋光检测器研究甲霜灵异构体在手性柱上的洗脱顺序;探讨进样浓度、进样流速、各区流速和切换时间等条件对手性分离甲霜灵外消旋体的影响,并与制备色谱进行比较。结果表明:S-(+)-甲霜灵先于R-(-)-甲霜灵被流动相洗脱,R-(-)-甲霜灵在色谱柱上的保留强于S-(+)-甲霜灵;在线性和非线性条件下,模拟移动床都能很好地拆分甲霜灵外消旋体,在优化SMB工艺条件下,S-(+)-甲霜灵和R-(-)-甲霜灵的光学纯度都大于99%;在样品质量浓度为15 mg/mL的条件下,模拟移动床色谱分离的样品量显著高于制备色谱,而流动相消耗仅为后者的1/9。这对于发展大规模色谱拆分甲霜灵工艺具有良好的指导意义。     

书刊征订

《制备色谱技术及应用》(第二版)(ISBN 978-7-122-11958-2)该书从色谱科学的角度详细地阐述了制备色谱的原理、重要的实验技术、关键性色谱分离技巧及其应用。内容包括制备色谱的基础知识、制备薄层色谱、常压柱色谱、低压及中压柱色谱、高压制备液相色谱、高速逆流色谱、模拟移动床色     

《制备色谱技术及应用》(第二版)

(ISBN 978-7-122-11958-2)该书从色谱科学的角度详细地阐述了制备色谱的原理、重要的实验技术、关键性色谱分离技巧及其应用。内容包括制备色谱的基础知识、制备薄层色谱、常压柱色谱、低压及中压柱色谱、高压制备液相色谱、高速逆流色谱、模拟移动床色谱、顶替色谱、制备气相色谱、电泳以及与制备色谱技术紧密相关的生物代谢产物的提取分离技术等。本书对制备色谱技术的系统介绍具有简明、系统、全面的特点。     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.