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CN103657152B - Novel separation system for simulated moving bed chromatography (SMBC) - Google Patents

Novel separation system for simulated moving bed chromatography (SMBC)
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CN103657152B
CN103657152BCN201310683807.5ACN201310683807ACN103657152BCN 103657152 BCN103657152 BCN 103657152BCN 201310683807 ACN201310683807 ACN 201310683807ACN 103657152 BCN103657152 BCN 103657152B
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宋峰
庄淑娟
傅忠君
黄昊飞
于鲁汕
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Nantong Yongsheng Chemical Co Ltd
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Shandong University of Technology
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Abstract

The invention discloses a novel separation system for a simulated moving bed chromatography (SMBC), and belongs to the technical field of chromatography separation. The separation system adopts a chromatographic column as an operation unit, and comprises N functional bands (N is not less than 5 and not greater than 7), two material inlets, three product outlets and 1-2 eluent inlets. The novel separation system for the simulated moving bed chromatography can be used for separation of mixture with three or more components and producing high-purity products by combination of a conventional simulated moving bed, so that the adsorbent and solvent consumption is reduced.

Description

Translated fromChinese
新型模拟移动床色谱分离系统New Simulated Moving Bed Chromatographic Separation System

技术领域technical field

本发明涉及一种新型模拟移动床色谱分离系统,属于色谱分离技术领域。The invention relates to a novel simulated moving bed chromatographic separation system, which belongs to the technical field of chromatographic separation.

背景技术Background technique

模拟移动床色谱是一种连续地色谱分离技术。它将多根色谱柱首尾相接,沿液相流动方向周期性切换物料进出口位置,实现液固两相之间的模拟逆流流动,以增加液固两相见的传质推动力,根本上提高了色谱分离效率。SMB最初主要应用于石化领域的C8分离和食品工业的糖类分离。因SMB最适于分离双组分,故在上世纪90年代被成功地引入到手性药物分离领域,获得广泛关注,SMB在双组分分离方面的原理与工艺优化等已被研究得十分深入和透彻。Simulated moving bed chromatography is a continuous chromatographic separation technique. It connects multiple chromatographic columns end to end, and periodically switches the position of the material inlet and outlet along the liquid phase flow direction to realize the simulated countercurrent flow between the liquid and solid phases, so as to increase the mass transfer driving force of the liquid and solid phases. Improved chromatographic separation efficiency. SMB was originally mainly used in the separation of C8 in the petrochemical field and the separation of sugars in the food industry. Because SMB is most suitable for the separation of two components, it was successfully introduced into the field of chiral drug separation in the 1990s and received widespread attention. The principle and process optimization of SMB in the separation of two components have been studied very deeply and thorough.

但在目前,模拟移动床色谱(Simulated moving bed chromatography,SMBC)的主要问题是只能将双组份的混合物分离为两个高纯度产品,或者将多组分混合物分离为含量不同的两部分混合物。如果对多组分混合物进行高纯度分离,需要进行多次分离,这样不仅仅延长了生产周期,还增大了溶剂,固定相的消耗。But at present, the main problem of simulated moving bed chromatography (SMBC) is that it can only separate two-component mixtures into two high-purity products, or separate multi-component mixtures into two-part mixtures with different contents. . If a multi-component mixture is separated with high purity, multiple separations are required, which not only prolongs the production cycle, but also increases the consumption of solvents and stationary phases.

发明内容Contents of the invention

本发明的目的是提供一种新型模拟移动床色谱分离系统,该系统可以从三组分混合物中分离出高纯度的三种组分的产品,并且可以与其它分离系统相结合能够从多组分混合物中分离出所有组分的高纯度产品。The purpose of this invention is to provide a novel simulated moving bed chromatographic separation system, which can separate high-purity three-component products from three-component mixtures, and can be combined with other separation systems to separate from multi-component A high purity product of all components is separated from the mixture.

本发明所述的新型模拟移动床分离系统是:以色谱柱为操作单元,由N个功能带组成,5≤N≤7,N为整数,并具有2个原料进口,3个产品出口和1-2个洗脱剂进口。The novel simulated moving bed separation system of the present invention is: the chromatographic column is used as the operating unit, and it is composed of N functional bands, 5≤N≤7, N is an integer, and has 2 raw material inlets, 3 product outlets and 1 - 2 eluent inlets.

其中:in:

1、当N=7时,该系统包括强保留组分洗脱带,强保留组分、中等保留组分的二次精制带,强保留组分、中等保留组分的一次精制带,中等保留组分富集洗脱带,中等保留组分、弱保留组分的二次精制带,中等保留组分、弱保留组分的一次精制带,弱保留组分富集带。1. When N=7, the system includes the elution band of strongly retained components, the secondary refining band of strongly retained components and moderately retained components, the primary refined band of strongly retained components and moderately retained components, and the moderately retained components Component enrichment elution band, secondary refining band of medium retention component and weak retention component, primary purification band of medium retention component and weak retention component, enrichment band of weak retention component.

(1)该系统具有一个洗脱剂进口时,用第一洗脱剂进口表示;(1) When the system has one eluent inlet, it is represented by the first eluent inlet;

第一原料进口位于强保留组分、中等保留组分的二次精制带与强保留组分、中等保留组分的一次精制带之间;The first raw material inlet is located between the secondary refining zone of strongly retained components and moderately retained components and the primary refining zone of strongly retained components and moderately retained components;

第二原料进口位于中等保留组分、弱保留组分的二次精制带与中等保留组分、弱保留组分的一次精制带之间;The second raw material inlet is located between the secondary refining zone of medium and weakly retained components and the primary refining zone of medium and weakly retained components;

第一产品出口位于强保留组分洗脱带与强保留组分、中等保留组分的二次精制带之间;The outlet of the first product is located between the elution band of strong retention components and the secondary refining band of strong retention components and medium retention components;

第二产品出口位于中等保留组分富集洗脱带与中等保留组分、弱保留组分的二次精制带之间;The second product outlet is located between the enrichment elution band of medium retention components and the secondary refining band of medium retention components and weak retention components;

第三产品出口位于中等保留组分、弱保留组分的一次精制带与弱保留组分富集带之间;The outlet of the third product is located between the primary refining zone of medium and weakly retained components and the enrichment zone of weakly retained components;

第一洗脱剂进口位于强保留组分洗脱带之前。The first eluent inlet is located before the elution band of strongly retained components.

(2)该系统具有两个洗脱剂进口,分别用第一洗脱剂进口,第二洗脱剂进口来表示;(2) The system has two eluent inlets, represented by the first eluent inlet and the second eluent inlet respectively;

第一原料进口位于强保留组分、中等保留组分的二次精制带与强保留组分、中等保留组分的一次精制带之间;The first raw material inlet is located between the secondary refining zone of strongly retained components and moderately retained components and the primary refining zone of strongly retained components and moderately retained components;

第二原料进口位于中等保留组分、弱保留组分的二次精制带与中等保留组分、弱保留组分的一次精制带之间;The second raw material inlet is located between the secondary refining zone of medium and weakly retained components and the primary refining zone of medium and weakly retained components;

第一产品出口位于强保留组分洗脱带与强保留组分、中等保留组分的二次精制带之间;The outlet of the first product is located between the elution band of strong retention components and the secondary refining band of strong retention components and medium retention components;

第二产品出口位于中等保留组分富集洗脱带与中等保留组分、弱保留组分的二次精制带之间;The second product outlet is located between the enrichment elution band of medium retention components and the secondary refining band of medium retention components and weak retention components;

第三产品出口位于中等保留组分、弱保留组分的一次精制带与弱保留组分富集带之间;The outlet of the third product is located between the primary refining zone of medium and weakly retained components and the enrichment zone of weakly retained components;

第一洗脱剂进口位于强保留组分洗脱带之前;The first eluent inlet is located before the strongly retained component elution band;

第二洗脱剂进口位于强保留组分、中等保留组分的一次精制带与中等保留组分富集洗脱带之间。The second eluent inlet is located between the strongly retained components, the primary refining band of the moderately retained components, and the enriched elution band of the moderately retained components.

2、当N=6时,该系统包括强保留组分洗脱带,强保留组分和中等保留组分的二次精制带,强保留组分和中等保留组分的一次精制带,中等保留组分富集洗脱带,中等保留组分和弱保留组分的二次精制带,中等保留组分和弱保留组分的一次精制带。2. When N=6, the system includes the elution band of strongly retained components, the secondary refining band of strongly retained components and moderately retained components, the primary refined band of strongly retained components and moderately retained components, and the moderately retained components Component-enriched elution bands, secondary refined bands of moderately retained components and weakly retained components, primary refined bands of moderately retained components and weakly retained components.

(1)该系统具有一个洗脱剂进口时,用第一洗脱剂进口表示;(1) When the system has one eluent inlet, it is represented by the first eluent inlet;

第一原料进口位于强保留组分、中等保留组分的二次精制带与强保留组分、中等保留组分的一次精制带之间;The first raw material inlet is located between the secondary refining zone of strongly retained components and moderately retained components and the primary refining zone of strongly retained components and moderately retained components;

第二原料进口位于中等保留组分、弱保留组分的二次精制带与中等保留组分、弱保留组分的一次精制带之间;The second raw material inlet is located between the secondary refining zone of medium and weakly retained components and the primary refining zone of medium and weakly retained components;

第一产品出口位于强保留组分洗脱带与强保留组分、中等保留组分的二次精制带之间;The outlet of the first product is located between the elution band of strong retention components and the secondary refining band of strong retention components and medium retention components;

第二产品出口位于中等保留组分富集洗脱带与中等保留组分、弱保留组分的二次精制带之间;The second product outlet is located between the enrichment elution band of medium retention components and the secondary refining band of medium retention components and weak retention components;

第三产品出口位于中等保留组分、弱保留组分的一次精制带之后;The outlet of the third product is located after the primary refining zone of medium retention components and weak retention components;

第一洗脱剂进口位于强保留组分洗脱带之前。The first eluent inlet is located before the elution band of strongly retained components.

(2)该系统具有两个洗脱剂进口,分别用第一洗脱剂进口,第二洗脱剂进口来表示;(2) The system has two eluent inlets, represented by the first eluent inlet and the second eluent inlet respectively;

第一原料进口位于强保留组分、中等保留组分的二次精制带与强保留组分、中等保留组分的一次精制带之间;The first raw material inlet is located between the secondary refining zone of strongly retained components and moderately retained components and the primary refining zone of strongly retained components and moderately retained components;

第二原料进口位于中等保留组分、弱保留组分的二次精制带与中等保留组分、弱保留组分的一次精制带之间;The second raw material inlet is located between the secondary refining zone of medium and weakly retained components and the primary refining zone of medium and weakly retained components;

第一产品出口位于强保留组分洗脱带与强保留组分、中等保留组分的二次精制带之间;The outlet of the first product is located between the elution band of strong retention components and the secondary refining band of strong retention components and medium retention components;

第二产品出口位于中等保留组分富集洗脱带与中等保留组分、弱保留组分的二次精制带之间;The second product outlet is located between the enrichment elution band of medium retention components and the secondary refining band of medium retention components and weak retention components;

第三产品出口位于中等保留组分、弱保留组分的一次精制带之后;The outlet of the third product is located after the primary refining zone of medium retention components and weak retention components;

第一洗脱剂进口位于强保留组分洗脱带之前;The first eluent inlet is located before the strongly retained component elution band;

第二洗脱剂进口位于强保留组分、中等保留组分的一次精制带与中等保留组分富集洗脱带之间。The second eluent inlet is located between the strongly retained components, the primary refining band of the moderately retained components, and the enriched elution band of the moderately retained components.

3、当N=5时,该系统包括强保留组分洗脱带,强保留组分和中等保留组分的二次精制带,强保留组分和中等保留组分的一次精制带,中等保留组分和弱保留组分的二次精制带,中等保留组分和弱保留组分的一次精制带。3. When N=5, the system includes the elution band of strongly retained components, the secondary refining band of strongly retained components and moderately retained components, the primary refined band of strongly retained components and moderately retained components, and the moderately retained Secondary refining bands for components and weakly retained components, primary refined bands for moderately retained components and weakly retained components.

(1)该系统具有一个洗脱剂进口时,用第一洗脱剂进口表示;(1) When the system has one eluent inlet, it is represented by the first eluent inlet;

第一原料进口位于强保留组分、中等保留组分的二次精制带与强保留组分、中等保留组分的一次精制带之间;The first raw material inlet is located between the secondary refining zone of strongly retained components and moderately retained components and the primary refining zone of strongly retained components and moderately retained components;

第二原料进口位于中等保留组分、弱保留组分的二次精制带与中等保留组分、弱保留组分的一次精制带之间;The second raw material inlet is located between the secondary refining zone of medium and weakly retained components and the primary refining zone of medium and weakly retained components;

第一产品出口位于强保留组分洗脱带与强保留组分、中等保留组分的二次精制带之间;The outlet of the first product is located between the elution band of strong retention components and the secondary refining band of strong retention components and medium retention components;

第二产品出口位于强保留组分、中等保留组分的一次精制带与中等保留组分、弱保留组分的二次精制带之间;The second product outlet is located between the primary refining zone of strongly retained components and moderately retained components and the secondary refining zone of moderately retained components and weakly retained components;

第三产品出口位于中等保留组分和弱保留组分的一次精制带之后;The third product outlet is located after the primary refining zone of medium retention components and weak retention components;

第一洗脱剂进口位于强保留组分洗脱带之前。The first eluent inlet is located before the elution band of strongly retained components.

(2)该系统具有两个洗脱剂进口,分别用第一洗脱剂进口,第二洗脱剂进口来表示;(2) The system has two eluent inlets, represented by the first eluent inlet and the second eluent inlet respectively;

第一原料进口位于强保留组分、中等保留组分的二次精制带与强保留组分、中等保留组分的一次精制带之间;The first raw material inlet is located between the secondary refining zone of strongly retained components and moderately retained components and the primary refining zone of strongly retained components and moderately retained components;

第二原料进口位于中等保留组分、弱保留组分的二次精制带与中等保留组分、弱保留组分的一次精制带之间;The second raw material inlet is located between the secondary refining zone of medium and weakly retained components and the primary refining zone of medium and weakly retained components;

第一产品出口位于强保留组分洗脱带与强保留组分、中等保留组分的二次精制带之间;The outlet of the first product is located between the elution band of strong retention components and the secondary refining band of strong retention components and medium retention components;

第二产品出口位于强保留组分、中等保留组分的一次精制带之后,中等保留组分、弱保留组分的二次精制带之前;The second product outlet is located after the primary refining zone of strongly retained components and moderately retained components, and before the secondary refining zone of moderately retained components and weakly retained components;

第三产品出口位于中等保留组分和弱保留组分的一次精制带之后;The third product outlet is located after the primary refining zone of medium retention components and weak retention components;

第一洗脱剂进口位于强保留组分洗脱带之前;The first eluent inlet is located before the strongly retained component elution band;

第二洗脱剂进口位于强保留组分、中等保留组分的一次精制带之后,中等保留组分、弱保留组分的二次精制带之前;且在第二产品出口之后。The second eluent inlet is located after the primary refining band of strongly retained components and moderately retained components, before the secondary refining band of moderately retained components and weakly retained components; and after the second product outlet.

该分离系统可以单独运行,也可以与其它的分离系统组合运行。其他分离系统可以为四带模拟移动床系统、改进的模拟移动床系统或萃取系统。The separation system can operate alone or in combination with other separation systems. Other separation systems can be four-band simulated moving bed systems, modified simulated moving bed systems or extraction systems.

本发明所述的三组分混合物和多组分混合物中分离出的组分均为保留性质不相同的组分。The components separated from the three-component mixture and the multi-component mixture in the present invention are all components with different retention properties.

本发明的有益效果如下:The beneficial effects of the present invention are as follows:

1、目前的模拟移动床系统,都是一个进料物流,只能得到1个或者2个高纯度的产品。本发明的新型模拟移动床分离系统可以同时进两个物流,含有三种组分,经分离后得到三种组分高纯度产品。1. The current simulated moving bed system is a feed stream, and only one or two high-purity products can be obtained. The novel simulated moving bed separation system of the present invention can feed two streams at the same time, containing three components, and obtain high-purity products of the three components after separation.

2、本发明的新型模拟移动床系统可以与其它系统结合,作为组合系统中的基本单元,分离多组分混合物原料,得到各种组分的高纯度产品。2. The novel simulated moving bed system of the present invention can be combined with other systems as a basic unit in the combined system to separate multi-component mixture raw materials and obtain high-purity products of various components.

附图说明Description of drawings

图1是实施例1中七带SMBC的结构示意图;Fig. 1 is the structural representation of seven band SMBC in embodiment 1;

图2是实施例2中七带SMBC的结构示意图;Fig. 2 is the structural representation of seven band SMBC in embodiment 2;

图3是实施例3中六带SMBC的结构示意图;Fig. 3 is the structural representation of six bands SMBC in embodiment 3;

图4是实施例4中六带SMBC的结构示意图;Fig. 4 is the structural representation of six bands SMBC in embodiment 4;

图5是实施例5中五带SMBC的结构示意图;Fig. 5 is the structural representation of five bands SMBC in embodiment 5;

图6是实施例6中五带SMBC的结构示意图;Fig. 6 is the structural representation of five bands SMBC in embodiment 6;

图7是实施例7中四带SMBC和七带SMBC组合连接结构示意图;Fig. 7 is four bands SMBC and seven bands SMBC combined connection structure schematic diagram in embodiment 7;

图8是实施例8中常规的四带模拟移动床色谱系统与本发明系统联合工作结构示意图。Fig. 8 is a schematic diagram of the combined working structure of the conventional four-band simulated moving bed chromatography system and the system of the present invention in Example 8.

具体实施方式Detailed ways

以下结合实施例对本发明作进一步描述。The present invention will be further described below in conjunction with embodiment.

实施例1Example 1

如图1所示,当N=7时,该系统包括强保留组分C洗脱带I,强保留组分C和中等保留组分B的二次精制带II,强保留组分C和中等保留组分B的一次精制带III,中等保留组分B富集洗脱带IV,中等保留组分B和弱保留组分A的二次精制带V,中等保留组分B和弱保留组分A的一次精制带VI,弱保留组分A富集带VII。As shown in Figure 1, when N=7, the system includes strongly retained component C elution band I, secondary refining band II of strongly retained component C and moderately retained component B, strongly retained component C and moderately Band III for the primary refinement of retained component B, enriched elution band IV for moderately retained fraction B, secondary refined band V for moderately retained fraction B and weakly retained fraction A, moderately retained fraction B and weakly retained fraction The primary refined band VI of A, and the weakly retained component A enriched band VII.

该系统具有一个洗脱剂进口,为第一洗脱剂进口D1;The system has one eluent inlet, being the first eluent inlet D1;

第一原料进口F1位于强保留组分C、中等保留组分B的二次精制带II与强保留组分C、中等保留组分B的一次精制带III之间;The first raw material inlet F1 is located between the secondary refining zone II of strongly retained component C and moderately retained component B and the primary refining zone III of strongly retained component C and moderately retained component B;

第二原料进口F2位于中等保留组分B、弱保留组分A的二次精制带V与中等保留组分B、弱保留组分A的一次精制带VI之间;The second raw material inlet F2 is located between the secondary refining zone V of medium retention component B and weak retention component A and the primary refining zone VI of medium retention component B and weak retention component A;

第一产品出口R1位于I带、II带之间;The first product export R1 is located between the I belt and the II belt;

第二产品出口RE位于IV带、V带之间;The second product outlet RE is located between the IV belt and the V belt;

第三产品出口E2位于VI带、VII带之间;The third product exit E2 is located between the VI zone and the VII zone;

第一洗脱剂进口D1位于I带之前。The first eluent inlet D1 is located before the I zone.

工作时,进料F1含有组分B和C,进料F2含有组分A和B。洗脱液D1从I带前进入系统洗脱组分C,洗脱下的组分一部分经R1采出,一部分进入II带,在II带中B,C组分被进一步分离;离开II带的组分B,C与混合进料F1中的B,C组分进入III带;B进入IV带,并和残留的B组分混合流出IV带,一部分经RE口采出,一部分进入V带;V带中A,B组分得到进一步分离;离开V带的A,B组分与进料F2混合,进入VI带;在VI带中,A,B组分进行分离,使得A组分一部分经E2口采出,一部分进入VII带。流动相溶剂,通过VII带,循环回流,与洗脱液D混合进入I带。In operation, feed F1 contains components B and C and feed F2 contains components A and B. The eluent D1 enters the system to elute component C from the front of the I band, part of the eluted components is extracted through R1, and part of it enters the II band, and the B and C components are further separated in the II band; Components B, C and the B and C components in the mixed feed F1 enter the III zone; B enters the IV zone, and mixes with the residual B component to flow out of the IV zone, part of which is extracted through the RE port, and part of it enters the V zone; The A and B components in the V zone are further separated; the A and B components leaving the V zone are mixed with the feed F2 and enter the VI zone; in the VI zone, the A and B components are separated, so that part of the A component passes through Extracted from the E2 port, part of it enters the VII zone. The mobile phase solvent passes through band VII, circulates back, and mixes with eluent D to enter band I.

经此过程,使得组分A,B,C被完全分离,得到高纯度的产品。Through this process, components A, B, and C are completely separated to obtain high-purity products.

实施例2Example 2

如图2所示,当N=7时,该系统包括强保留组分C洗脱带I,强保留组分C和中等保留组分B的二次精制带II,强保留组分C和中等保留组分B的一次精制带III,中等保留组分B富集洗脱带IV,中等保留组分B和弱保留组分A的二次精制带V,中等保留组分B和弱保留组分A的一次精制带VI,弱保留组分A富集带VII。As shown in Figure 2, when N=7, the system includes strongly retained component C elution band I, secondary refining band II of strongly retained component C and moderately retained component B, strongly retained component C and moderately Band III for the primary refinement of retained component B, enriched elution band IV for moderately retained fraction B, secondary refined band V for moderately retained fraction B and weakly retained fraction A, moderately retained fraction B and weakly retained fraction The primary refined band VI of A, and the weakly retained component A enriched band VII.

该系统具有两个洗脱剂进口,分别为第一洗脱剂进口D1,第二洗脱剂进口D2;The system has two eluent inlets, namely the first eluent inlet D1 and the second eluent inlet D2;

第一原料进口F1位于强保留组分C、中等保留组分B的二次精制带II与强保留组分C、中等保留组分B的一次精制带III之间;The first raw material inlet F1 is located between the secondary refining zone II of strongly retained component C and moderately retained component B and the primary refining zone III of strongly retained component C and moderately retained component B;

第二原料进口F2位于中等保留组分B、弱保留组分A的二次精制带V与中等保留组分B、弱保留组分A的一次精制带VI之间;The second raw material inlet F2 is located between the secondary refining zone V of medium retention component B and weak retention component A and the primary refining zone VI of medium retention component B and weak retention component A;

第一产品出口R1位于I带、II带之间;The first product export R1 is located between the I belt and the II belt;

第二产品出口RE位于IV带、V带之间;The second product outlet RE is located between the IV belt and the V belt;

第三产品出口E2位于VI带、VII带之间;The third product exit E2 is located between the VI zone and the VII zone;

第一洗脱剂进口D1位于I带之前;The first eluent inlet D1 is located before the I zone;

第二洗脱剂进口D2位于III带、IV带之间。The second eluent inlet D2 is located between zone III and zone IV.

工作时,进料F1含有组分B和C,F2含有组分A和B。洗脱液D1从I带前进入系统洗脱组分C,洗脱下的组分一部分经R1采出,一部分进入II带,在II带中B,C组分被进一步分离;离开II带的组分B,C与混合进料F1中的B,C组分进入III带;B组分离开III带和洗脱液D2混合进入IV带,并和残留的B组分混合流出IV带,一部分经RE口采出,一部分进入V带;V带中A,B组分得到进一步分离;离开V带的A,B组分与进料F2混合,进入VI带;在VI带中,A,B组分进行分离,使得A组分一部分经E2口采出,一部分进入VII带。流动相溶剂,通过VII带,循环回流,与洗脱液D混合进入I带。In operation, feed F1 contains components B and C and F2 contains components A and B. The eluent D1 enters the system to elute component C from the front of the I band, part of the eluted components is extracted through R1, and part of it enters the II band, and the B and C components are further separated in the II band; Components B, C and the B and C components in the mixed feed F1 enter the III zone; the B component leaves the III zone and the eluent D2 mixes into the IV zone, and mixes with the residual B component to flow out of the IV zone, a part Extracted through the RE port, part of it enters the V zone; the A and B components in the V zone are further separated; the A and B components leaving the V zone are mixed with the feed F2 and enter the VI zone; in the VI zone, A, B The components are separated so that part of the A component is extracted through the E2 port, and part of it enters the VII zone. The mobile phase solvent passes through band VII, circulates back, and mixes with eluent D into band I.

经此过程,使得组分A,B,C被完全分离,得到高纯度的产品。Through this process, components A, B, and C are completely separated to obtain high-purity products.

实施例3Example 3

如图3所示,当N=6时,该系统包括强保留组分C洗脱带I,强保留组分C和中等保留组分B的二次精制带II,强保留组分C和中等保留组分B的一次精制带III,中等保留组分B富集洗脱带IV,中等保留组分B和弱保留组分A的二次精制带V,中等保留组分B和弱保留组分A的一次精制带VI。As shown in Figure 3, when N=6, the system includes strongly retained component C elution band I, secondary refining band II of strongly retained component C and moderately retained component B, strongly retained component C and moderately Band III for the primary refinement of retained component B, enriched elution band IV for moderately retained fraction B, secondary refined band V for moderately retained fraction B and weakly retained fraction A, moderately retained fraction B and weakly retained fraction A's primary refinement band VI.

该系统具有一个洗脱剂进口,为第一洗脱剂进口D1;The system has one eluent inlet, being the first eluent inlet D1;

第一原料进口F1位于强保留组分C、中等保留组分B的二次精制带II与强保留组分C、中等保留组分B的一次精制带III之间;The first raw material inlet F1 is located between the secondary refining zone II of strongly retained component C and moderately retained component B and the primary refining zone III of strongly retained component C and moderately retained component B;

第二原料进口F2位于中等保留组分B、弱保留组分A的二次精制带V与中等保留组分B、弱保留组分A的一次精制带VI之间;The second raw material inlet F2 is located between the secondary refining zone V of medium retention component B and weak retention component A and the primary refining zone VI of medium retention component B and weak retention component A;

第一产品出口R1位于I带、II带之间;The first product export R1 is located between the I belt and the II belt;

第二产品出口RE位于IV带、V带之间;The second product outlet RE is located between the IV belt and the V belt;

第三产品出口E2位于VI带之后;The third product exit E2 is located after the VI zone;

第一洗脱剂进口D1位于I带之前。The first eluent inlet D1 is located before the I zone.

工作时,进料F1含有组分B和C,F2含有组分A和B。洗脱液D1从I带前进入系统洗脱组分C,洗脱下的组分一部分经R1采出,一部分进入II带,在II带中B,C组分被进一步分离;离开II带的组分B,C与混合进料F1中的B,C组分进入III带;B进入IV带,并和残留的B组分混合流出IV带,一部分经RE口采出,一部分进入V带;V带中A,B组分得到进一步分离;离开V带的A,B组分与进料F2混合,进入VI带;在VI带中,A,B组分进行分离,使得A组分一部分经E2口采出。其余的A组分保留在吸附剂中进入下一个分离阶段。In operation, feed F1 contains components B and C and F2 contains components A and B. The eluent D1 enters the system to elute component C from the front of the I band, part of the eluted components is extracted through R1, and part of it enters the II band, and the B and C components are further separated in the II band; Components B, C and the B and C components in the mixed feed F1 enter the III zone; B enters the IV zone, and mixes with the residual B component to flow out of the IV zone, part of which is extracted through the RE port, and part of it enters the V zone; The A and B components in the V zone are further separated; the A and B components leaving the V zone are mixed with the feed F2 and enter the VI zone; in the VI zone, the A and B components are separated, so that part of the A component passes through Extracted from mouth E2. The rest of the A component remains in the adsorbent for the next separation stage.

经此过程,使得组分A,B,C被完全分离,得到高纯度的产品。Through this process, components A, B, and C are completely separated to obtain high-purity products.

实施例4Example 4

如图4所示,当N=6时,该系统包括强保留组分C洗脱带I,强保留组分C和中等保留组分B的二次精制带II,强保留组分C和中等保留组分B的一次精制带III,中等保留组分B富集洗脱带IV,中等保留组分B和弱保留组分A的二次精制带V,中等保留组分B和弱保留组分A的一次精制带VI。As shown in Figure 4, when N=6, the system includes strongly retained component C elution band I, secondary refining band II of strongly retained component C and moderately retained component B, strongly retained component C and moderately Band III for the primary refinement of retained component B, enriched elution band IV for moderately retained fraction B, secondary refined band V for moderately retained fraction B and weakly retained fraction A, moderately retained fraction B and weakly retained fraction A's primary refinement band VI.

该系统具有两个洗脱剂进口,分别为第一洗脱剂进口D1,第二洗脱剂进口D2;The system has two eluent inlets, namely the first eluent inlet D1 and the second eluent inlet D2;

第一原料进口F1位于强保留组分C、中等保留组分B的二次精制带II与强保留组分C、中等保留组分B的一次精制带III之间;The first raw material inlet F1 is located between the secondary refining zone II of strongly retained component C and moderately retained component B and the primary refining zone III of strongly retained component C and moderately retained component B;

第二原料进口F2位于中等保留组分B、弱保留组分A的二次精制带V与中等保留组分B、弱保留组分A的一次精制带VI之间;The second raw material inlet F2 is located between the secondary refining zone V of medium retention component B and weak retention component A and the primary refining zone VI of medium retention component B and weak retention component A;

第一产品出口R1位于I带、II带之间;The first product export R1 is located between the I belt and the II belt;

第二产品出口RE位于IV带、V带之间;The second product outlet RE is located between the IV belt and the V belt;

第三产品出口E2位于VI带之后;The third product exit E2 is located after the VI zone;

第一洗脱剂进口D1位于I带之前;The first eluent inlet D1 is located before the I zone;

第二洗脱剂进口D2位于III带、IV带之间。The second eluent inlet D2 is located between zone III and zone IV.

工作时,进料F1含有组分B和C,F2含有组分A和B。洗脱液D1从I带前进入系统洗脱组分C,洗脱下的组分一部分经R1采出,一部分进入II带,在II带中B,C组分被进一步分离;离开II带的组分B,C与混合进料F1中的B,C组分进入III带;B组分离开III带和洗脱液D2混合进入IV带,并和残留的B组分混合流出IV带,一部分经RE口采出,一部分进入V带;V带中A,B组分得到进一步分离;离开V带的A,B组分与进料F2混合,进入VI带;在VI带中,A,B组分进行分离,使得A组分一部分经E2口采出。其余的A组分保留在吸附剂中进入下一个分离阶段。In operation, feed F1 contains components B and C and F2 contains components A and B. The eluent D1 enters the system to elute component C from the front of the I band, part of the eluted components is extracted through R1, and part of it enters the II band, and the B and C components are further separated in the II band; Components B, C and the B and C components in the mixed feed F1 enter the III zone; the B component leaves the III zone and the eluent D2 mixes into the IV zone, and mixes with the residual B component to flow out of the IV zone, a part Extracted through the RE port, part of it enters the V zone; the A and B components in the V zone are further separated; the A and B components leaving the V zone are mixed with the feed F2 and enter the VI zone; in the VI zone, A, B The components are separated so that part of the A component is extracted through the E2 port. The rest of the A component remains in the adsorbent for the next separation stage.

经此过程,使得组分A,B,C被完全分离,得到高纯度的产品。Through this process, components A, B, and C are completely separated to obtain high-purity products.

实施例5Example 5

如图5所示,当N=5时,该系统包括强保留组分C洗脱带I,强保留组分C和中等保留组分B的二次精制带II,强保留组分C和中等保留组分B的一次精制带III,中等保留组分B和弱保留组分A的二次精制带V,中等保留组分B和弱保留组分A的一次精制带VI。As shown in Figure 5, when N=5, the system includes strongly retained component C elution band I, secondary refining band II of strongly retained component C and moderately retained component B, strongly retained component C and moderately The primary refining band III retained component B, the secondary refining band V contained moderately retained component B and weakly retained component A, and the primary refined band VI contained moderately retained component B and weakly retained component A.

该系统具有两个洗脱剂进口,分别为第一洗脱剂进口D1,第二洗脱剂进口D2;The system has two eluent inlets, namely the first eluent inlet D1 and the second eluent inlet D2;

第一原料进口F1位于强保留组分C、中等保留组分B的二次精制带II与强保留组分C、中等保留组分B的一次精制带III之间;The first raw material inlet F1 is located between the secondary refining zone II of strongly retained component C and moderately retained component B and the primary refining zone III of strongly retained component C and moderately retained component B;

第二原料进口F2位于中等保留组分B、弱保留组分A的二次精制带V与中等保留组分B、弱保留组分A的一次精制带VI之间;The second raw material inlet F2 is located between the secondary refining zone V of medium retention component B and weak retention component A and the primary refining zone VI of medium retention component B and weak retention component A;

第一产品出口R1位于I带、II带之间;The first product export R1 is located between the I belt and the II belt;

第二产品出口RE位于III带之后;The second product exit RE is located after zone III;

第三产品出口E2位于VI带之后;The third product exit E2 is located after the VI zone;

第一洗脱剂进口D1位于I带之前;The first eluent inlet D1 is located before the I zone;

第二洗脱剂进口D2位于V带之前。III带和V带断开。The second eluent inlet D2 is located before the V-belt. The III belt and the V belt are disconnected.

工作时,进料F1含有组分B和C,F2含有组分A和B。洗脱液D1从I带前进入系统洗脱组分C,洗脱下的组分一部分经R1采出,一部分进入II带,在II带中B,C组分被进一步分离;离开II带的组分B,C与混合进料F1中的B,C组分进入III带;B组分离开III带,经RE口采出;III带和V带断开;洗脱液D2在V带前进入系统,使得组分A,B得到进一步分离;离开V带的A,B组分与进料F2混合,进入VI带;在VI带中,A,B组分进行分离,使得A组分一部分经E2口采出。其余的A组分保留在吸附剂中进入下一个分离阶段。In operation, feed F1 contains components B and C and F2 contains components A and B. The eluent D1 enters the system to elute component C from the front of the I band, part of the eluted components is extracted through R1, and part of it enters the II band, and the B and C components are further separated in the II band; Components B, C and B and C components in the mixed feed F1 enter the III zone; B components leave the III zone and are extracted through the RE port; the III zone and the V zone are disconnected; the eluent D2 is in front of the V zone Entering the system, the components A and B are further separated; the A and B components leaving the V zone are mixed with the feed F2 and enter the VI zone; in the VI zone, the A and B components are separated, so that a part of the A component Extracted through mouth E2. The rest of the A component remains in the adsorbent for the next separation stage.

经此过程,使得组分A,B,C被完全分离,得到高纯度的产品。Through this process, components A, B, and C are completely separated to obtain high-purity products.

实施例6Example 6

如图6所示,当N=5时,该系统包括强保留组分C洗脱带I,强保留组分C和中等保留组分B的二次精制带II,强保留组分C和中等保留组分B的一次精制带III,中等保留组分B和弱保留组分A的二次精制带V,中等保留组分B和弱保留组分A的一次精制带VI。As shown in Figure 6, when N=5, the system includes strongly retained component C elution band I, secondary refining band II of strongly retained component C and moderately retained component B, strongly retained component C and moderately The primary refining band III retained component B, the secondary refining band V contained moderately retained component B and weakly retained component A, and the primary refined band VI contained moderately retained component B and weakly retained component A.

该系统具有一个洗脱剂进口,为第一洗脱剂进口D1;The system has one eluent inlet, being the first eluent inlet D1;

第一原料进口F1位于强保留组分C、中等保留组分B的二次精制带II与强保留组分C、中等保留组分B的一次精制带III之间;The first raw material inlet F1 is located between the secondary refining zone II of strongly retained component C and moderately retained component B and the primary refining zone III of strongly retained component C and moderately retained component B;

第二原料进口F2位于中等保留组分B、弱保留组分A的二次精制带V与中等保留组分B、弱保留组分A的一次精制带VI之间;The second raw material inlet F2 is located between the secondary refining zone V of medium retention component B and weak retention component A and the primary refining zone VI of medium retention component B and weak retention component A;

第一产品出口R1位于I带、II带之间;The first product export R1 is located between the I belt and the II belt;

第二产品出口RE位于III带、V带之间;The second product export RE is located between the III belt and the V belt;

第三产品出口E2位于VI带之后;The third product exit E2 is located after the VI zone;

第一洗脱剂进口D1位于I带之前。The first eluent inlet D1 is located before the I zone.

工作时,进料F1含有组分B和C,F2含有组分A和B。洗脱液D1从I带前进入系统洗脱组分C,洗脱下的组分一部分经R1采出,一部分进入II带,在II带中B,C组分被进一步分离;离开II带的组分B,C与混合进料F1中的B,C组分进入III带;B组分离开III带,一部分经RE口采出,一部分进入V带;V带中组分A,B得到进一步分离;离开V带的A,B组分与进料F2混合,进入VI带;在VI带中,A,B组分进行分离,使得A组分一部分经E2口采出。其余的A组分保留在吸附剂中进入下一个分离阶段。In operation, feed F1 contains components B and C and F2 contains components A and B. The eluent D1 enters the system to elute component C from the front of the I band, part of the eluted components is extracted through R1, and part of it enters the II band, and the B and C components are further separated in the II band; Components B, C and the B and C components in the mixed feed F1 enter the III zone; B components leave the III zone, part of which is extracted through the RE port, and part of it enters the V zone; the components A and B in the V zone are further Separation; A and B components leaving V zone are mixed with feed F2 and enter VI zone; in VI zone, A and B components are separated, so that part of A component is extracted through E2 port. The rest of the A component remains in the adsorbent for the next separation stage.

经此过程,使得组分A,B,C被完全分离,得到高纯度的产品。Through this process, components A, B, and C are completely separated to obtain high-purity products.

实施例7Example 7

如图7所示,四带模拟移动床色谱系统中,进料F含有组分A,B和C。经过四带模拟移动床色谱分离后,分别得到含有组分B和C的混合液R和含有组分A和B的混合液E。R溶液可以作为七带模拟移动床色谱的进料F1,E溶液可以作为F2,七带模拟移动床色谱的运行方式为实施例1中的系统。As shown in Figure 7, feed F contains components A, B and C in a four-band simulated moving bed chromatography system. After four-band simulated moving bed chromatographic separation, the mixed solution R containing components B and C and the mixed solution E containing components A and B were obtained respectively. The R solution can be used as the feed F1 of the seven-band simulated moving bed chromatography, the E solution can be used as F2, and the operating mode of the seven-band simulated moving bed chromatography is the system in Example 1.

两个系统互相关联同时运作,也可以设置E,R的缓冲槽,使两个系统单独运行,以增强系统鲁棒性。The two systems are interrelated and operate simultaneously, and the buffer tanks of E and R can also be set to make the two systems operate independently to enhance the robustness of the system.

实施例8Example 8

如图8所示,进料F中含有A,B,C,D,E,F,G七种组分。以常规的四带模拟移动床色谱系统和本发明提出的新型模拟移动床色谱系统为基本单元,可以得到一套分离七组分混合物,得到全部高纯度产品的工作流程图。As shown in Figure 8, feed F contains seven components A, B, C, D, E, F, and G. Using the conventional four-band simulated moving bed chromatographic system and the novel simulated moving bed chromatographic system proposed by the present invention as basic units, a set of work flow diagrams for separating seven-component mixtures and obtaining all high-purity products can be obtained.

实施例9Example 9

以丁醇、戊醇和己醇组成的三元混合物为原料,以键合C18的硅胶填料为固定相,流动相(体积比)组成为甲醇:水=2:8。根据本发明实施例1提出的模拟移动床运行结构,进行模拟移动床色谱分离,在三个产品出口分别得到三种产品,其中R1出口中,己醇质量百分含量为99.96%,丁醇质量百分含量为0.002%,戊醇质量百分含量为0.038%;RE出口中,己醇质量百分含量为0.03%,丁醇质量百分含量为0.05%,戊醇质量百分含量为99.92%;E2出口中,己醇质量百分含量为0.005%,丁醇质量百分含量为99.945%,戊醇质量百分含量为0.05%。The ternary mixture composed of butanol, pentanol and hexanol is used as the raw material, the C18-bonded silica gel filler is used as the stationary phase, and the mobile phase (volume ratio) is composed of methanol:water=2:8. According to the simulated moving bed operating structure proposed in Embodiment 1 of the present invention, simulated moving bed chromatographic separation is carried out, and three products are obtained respectively at three product outlets, wherein in the R1 outlet, the mass percentage of hexanol is 99.96%, and the mass percentage of butanol is 99.96%. The percentage content is 0.002%, the mass percentage content of pentanol is 0.038%; in the export of RE, the mass percentage content of hexanol is 0.03%, the mass percentage content of butanol is 0.05%, and the mass percentage content of pentanol is 99.92% ; In the export of E2, the mass percentage of hexanol is 0.005%, the mass percentage of butanol is 99.945%, and the mass percentage of amyl alcohol is 0.05%.

以上实施例是对专利的说明和进一步解释,而不是对本发明的限制,在本发明的精神和权利保护范围内所做的任何修改,都落入本发明的保护范围。The above embodiments are descriptions and further explanations of the patents, rather than limitations to the present invention, and any modifications made within the spirit and scope of protection of the present invention all fall within the protection scope of the present invention.

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CN101177716A (en)*2007-12-122008-05-14江南大学 A method for separating and purifying glucose, fructose and polyoligosaccharides from fructose syrup
EP2418009A1 (en)*2009-04-082012-02-15Universidade Do PortoSimulated moving bed membrane reactor, new hybrid separation process and uses thereof
CN102924538A (en)*2012-10-312013-02-13江南大学Method for extracting xylose, arabinose and galactose from xylose fermentation broth or xylose mother liquor

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