CN1598568A - Array continuous preparing chromatography system and using method thereof - Google Patents
Array continuous preparing chromatography system and using method thereof Download PDFInfo
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- CN1598568A CN1598568A CN 03146864 CN03146864A CN1598568A CN 1598568 A CN1598568 A CN 1598568A CN 03146864 CN03146864 CN 03146864 CN 03146864 A CN03146864 A CN 03146864A CN 1598568 A CN1598568 A CN 1598568A
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Abstract
The invention discloses an array style continuous preparation chromatogram system and its using method, the system includes separating part, material transporting part, solvent transporting part, collecting part and controlling part, and the separating part includes array chromatogram column, which is composed of at least two chromatogram columns. When continuously and equably sending into the array chromatogram columns, the feed-in controlling valve is controlled by the controlling computer and controlling closet, simulating circular chromatogram feed-in style switching in turn, periodically, equably feed-in to each chromatogram column, the purging product is collected by special collecting equipment of array chromatogram, controlled by the controlling part, then sending them to the products storing container. The system is suitable to several group continuous large-scale preparation.
Description
Technical field
The present invention relates to the continuous preparative chromatography of extensive polycomponent system field, relate in particular to the continuous preparative chromatography of array system field.
Background technology
Chromatographic technique is the different technical systems that make that each component in the potpourri is separated from each other of retention time that causes by the acting force difference of material between two-phase.Chromatogram can be divided into AG chromatogram and preparation scale chromatogram again by its purposes.The former has the very low lower limit that detects, and can detect the trace components that contains in the potpourri, is mainly used in material and identifies; The latter is mainly used in the separation of effective constituent in the material and purifies, and is suitable for scale preparation and suitability for industrialized production.Preparative chromatography can be divided into intermittently operated and continued operation again by its mode of operation.The packed column chromatogram is the former typical case's representative, and its advantage is to be suitable for multi-component separation, and is easy to amplify.But the packed column chromatogram can only intermittently operated, is not suitable for large-scale continuous commercial production.Widely used continuous preparative chromatography mainly is simulated moving bed chromatography and annular chromatography at present.The ultimate principle of simulated moving bed chromatography (with reference to Chinese patent CN1126628A and CN1374146A) is to keep adsorbent bed motionless, simulates the similar staggered effect that flows by continuous change liquid in-out mouth.This chromatogram is amplified easily, realizes operation automation easily, but only is applicable to the separation of two component systems usually.The ultimate principle of ring-type rotation chromatogram (with reference to Chinese patent CN1307679A) is that moving phase is flow through from the double-layered cylinder that adsorbent is housed continuously, and material liquid is from the dispensing head outflow of top rotation, self gravity move downward and the stack of the circular motion that rotates under, material liquid is done scroll along wall and is moved, and just can obtain different separation components in the different fixing position of cylinder bottom like this.Annular chromatography is suitable for the separation of many components system, but amplify difficulty, and relate to that the motive seal problem of pressure-containing member and solute produce radial diffusion in the cylindrical wall moving process and the product that causes is impure, so that the difficulty of the actual popularization of this chromatographic technique is bigger.
Summary of the invention
The object of the present invention is to provide a kind of preparative chromatography system that is suitable for many components, extensive, serialization requirement.This system has broken through the restriction that simulated moving bed chromatography can only be separated two component systems; Overcome the motive seal and the solute diffusion problem of ring-type rotation chromatogram, and be easy to amplify.
The continuous preparative chromatography of array of the present invention system, adopt similar simulation moving-bed control method, come the bed on the realization theory to move by the control feed points, and actual bed is motionless, promptly realize the theoretic rotation of annular bed, thereby avoid the motive seal problem of liquor inlet by the feed points of control circular chromatography; And a plurality of chromatographic columns that adopt ring shooting substitute the annular bed of circular chromatography as the unit separation equipment, avoided the diffusion of solute, not only be suitable for the separation of many components system, and amplified easily at circumferencial direction, technology is also ripe, can adapt to the production requirement of different scales.In the practical application, chromatographic column needn't can be lined up chromatographic column array arbitrarily by ring shooting.
The continuous preparative chromatography of array provided by the invention system comprises:
Separating part comprises that, quantity identical by specification is the array chromatographic column that 2 or above chromatographic column are formed;
The solvent delivery part comprises solvent storage container, solvent pump and solvent control main valve, and described solvent storage container, solvent pump and solvent control main valve are connected successively by pipeline, links to each other with the top inlet of each post of array chromatographic column respectively by pipeline again;
The raw material transport portion, comprise that raw material storage container, feeder pump, charging control main valve and charging control divide valve, described raw material storage container, feeder pump and charging control main valve are connected successively by pipeline, divide the pipeline of valve to link to each other with the top inlet of each post of array chromatographic column respectively by being equipped with charging control again;
Collect part, comprise array chromatogram special product gatherer and product storage container, described array chromatogram special product gatherer is used for collecting the wash-out product that flows out from each post of array chromatographic column, and this array chromatogram special product gatherer inlet links to each other with the eluent export pipeline that is equipped with flow control valve of each post bottom of array chromatographic column; Described product storage container links to each other with the outlet of array chromatogram special product gatherer by pipeline, is used to store each wash-out product of collecting;
Control section, comprise computing machine and switch board, described computing machine links to each other with switch board, described switch board divides valve, array chromatogram special product gatherer to link to each other with charging control, establish array chromatogram control program software in the computing machine, by switch board control a feeding manner that each charging control divides valve simulation circular chromatography switch successively ground, periodically, equably to each the post charging of array chromatographic column, and the wash-out product is collected by array of controls chromatogram special product gatherer.
Another object of the present invention is to provide the using method of the continuous preparative chromatography of array system.In the continuous preparative chromatography of array provided by the invention system, solvent (being eluent) is sent into each post of array chromatographic column of separating part equably by the solvent delivery partial continuous, charging control by control raw material importation simultaneously divides valve, make material liquid to be separated periodically enter each post of array chromatographic column, if the post number of array chromatographic column is n, when then n post being circulated sample introduction, cycle period should equal the sample introduction cycle and product is collected period T
pThe sample injection time that each post is shared is the longest at interval to be T
p/ n.Like this, the sample introduction t zero hour of i post
S, iFor:
t
S, i=(i-1) T
p/ n+ (k-1) T
p(i=1,2 ..., n; K=1,2 ...) in the formula, k is a period.Sample introduction finish time of i post is the sample introduction zero hour of (i+1) post just.
If control the flow of sample introduction pipeline and each sample size well, and when n is enough big, just may make total system look like continuous operation from the outside.The post of array chromatographic column is counted n and is at least 2, does not limit at most.Obviously, the number of chromatographic column is many more, and the distribution of chromatographic band just approaches annular bed more.Consider practical application, its quantitative range may be selected to be 2～100, also can be some more more as required, and preferable range is 20～100.
As the preferred version of system of the present invention, the preferred volume pump of feedstock pump and solvent pump.Switch board links to each other with solvent pump with this feedstock pump respectively, and they are controlled.
For realizing serialization and robotization fully, operate simplyr, can be further the switch board of control section be linked to each other with solvent control main valve, charging control main valve respectively, and they are controlled.
As the preferred version of system of the present invention, can also in each post eluent export pipeline of array chromatographic column, flowmeter be set, whether convenient each post flow of monitoring is consistent.
Charging control divides preferably solenoid valve of valve, by computer program control each charging control divide valve the suitable time to each chromatographic column charging, the feeding manner of promptly simulating circular chromatography switch successively, periodically, equably to each the post charging of array chromatographic column.
In system of the present invention, the optional hand valve of described flow control valve also can be selected motorized valve, and purpose is that the solvent flux of guaranteeing each chromatographic column is consistent.Another kind of selectable scheme is: flow control valve is a motorized valve, flowmeter is the flowmeter of belt sensor, this flowmeter is connected with switch board respectively with flow control valve, comes the Control Flow control valve by computing machine according to the transducing signal of flowmeter, guarantees each post flow unanimity.
Description of drawings
Fig. 1 is a system embodiment synoptic diagram of the present invention.
Embodiment
The invention will be further described below in conjunction with drawings and Examples.See Fig. 1, the embodiment of the continuous preparative chromatography of array of the present invention system comprises:
Array chromatographic column 1 is that 20-100 the identical chromatographic column of specification formed by quantity;
Solvent storage container 9, solvent pump 4, solvent control main valve 41, wherein, solvent storage container 9, solvent pump 4 and solvent control main valve 41 are connected successively by pipeline, link to each other with the top inlet of array chromatographic column 1 each post by pipeline respectively again;
Raw material storage container 10, feedstock pump 3, charging control main valve 31, wherein, described raw material storage container 10, feedstock pump 3 and charging control main valve 31 are connected successively by pipeline, divide the pipeline of valve 6 to link to each other with the top inlet of array chromatographic column 1 each post by being equipped with charging control respectively again, it is solenoid valves that this charging control divides valve 6;
Array chromatogram special product gatherer 2 and product storage container 5, wherein, the inlet of array chromatogram special product gatherer 2 connects the eluent export pipeline that is equipped with flow control valve 7 and flowmeter 8 of array chromatographic column 1 each post bottom, product storage container 5 links to each other with each outlet of array chromatogram special product gatherer 2 by pipeline, and flow control valve 7 is a hand valve;
Among this embodiment, described array chromatographic column is made up of the identical 30-100 of a specification chromatographic column, the charging of each chromatographic column divides valve 6 to control by charging control, charging control divide valve 6 by computing machine 11 according to predefined array chromatogram control program software, control by switch board 12, to guarantee that each chromatographic column is at suitable time sample introduction, the solvent flux of each chromatographic column is consistent, the wash-out product is collected by array chromatogram special product gatherer 2, delivers to respectively in each product storage container 5.
Experiment:
1. make an array preparative chromatography system that 32 root chromatogram columns are arranged, chromatographic column is a silica gel H, 10～40 μ m, and 50mm * 300mm has 64 liquid baths on the distribution plate of its array chromatogram product special collector, can collect 64 products at most.
2. ginkalide A, ginkolide B separate with the Bilobalide ternary mixture:
Adopting ethyl acetate/petroleum ether (volume ratio=8: 2) is solvent (moving phase).With moving phase potpourri is dissolved, as material liquid.Start solvent pump, be 10ml/min with the flow velocity of each post of flow regulation valve regulation.Recording cycle period through the single-column test is 256 minutes, so the sample injection time of each post is spaced apart 256/32=8 minute.Start array chromatogram special product gatherer, the product collection cycle is set at 256 minutes, label is that 1 liquid bath forwards the following time of drain pipe that is positioned at first post on distribution plate, picks up counting, and gives the first post sample introduction, switch to the second post sample introduction in the time of the 8th minute, switch to the 3rd post sample introduction in the time of the 16th minute ..., in the time of the 256th minute, circulation is taken turns in beginning second, so analogizes.The switching of sample introduction is controlled by computing machine fully.
After preparation is finished, with high performance liquid chromatography the sample in 64 product receiving flasks is analyzed, the result is: the product in 20～No. 24 bottles mainly contains ginkalide A, and purity is greater than 98%; Product in 28～No. 38 bottles mainly contains ginkolide B, and purity is greater than 98%; Product in 48～No. 64 bottles mainly contains Bilobalide, and purity is greater than 98%; Liquid in all the other each product receiving flasks mainly is solvent (moving phase).
Claims (10)
1. the continuous preparative chromatography of array system is used for the continuous large-scale preparation of polycomponent product, and this system comprises:
Separating part comprises that, quantity identical by specification is the array chromatographic column that 2 or above chromatographic column are formed;
The solvent delivery part comprises solvent storage container, solvent pump and solvent control main valve, and described solvent storage container, solvent pump and solvent control main valve are connected successively by pipeline, links to each other with the top inlet of each post of array chromatographic column respectively by pipeline again;
The raw material transport portion, comprise that raw material storage container, feeder pump, charging control main valve and charging control divide valve, described raw material storage container, feeder pump and charging control main valve are connected successively by pipeline, divide the pipeline of valve to link to each other with the top inlet of each post of array chromatographic column respectively by being equipped with charging control again;
Collect part, comprise array chromatogram special product gatherer and product storage container, described array chromatogram special product gatherer is used for collecting the wash-out product that flows out from each post of array chromatographic column, and this array chromatogram special product gatherer inlet links to each other with the eluent export pipeline that is equipped with flow control valve of each post bottom of array chromatographic column; Described product storage container links to each other with the outlet of array chromatogram special product gatherer by pipeline, is used to store each wash-out product of collecting;
Control section, comprise computing machine and switch board, described computing machine links to each other with switch board, described switch board divides valve, array chromatogram special product gatherer to link to each other with charging control, establish array chromatogram control program software in the computing machine, by switch board control a feeding manner that each charging control divides valve simulation circular chromatography switch successively ground, periodically, equably to each the post charging of array chromatographic column, and the wash-out product is collected by array of controls chromatogram special product gatherer.
2. according to the continuous preparative chromatography of the described array of claim 1 system, it is characterized in that: the post quantitative range of described array chromatographic column is 20-100.
3. according to the continuous preparative chromatography of the described array of claim 1 system, it is characterized in that: it is solenoid valve that described charging control divides valve.
4. according to the continuous preparative chromatography of the described array of claim 1 system, it is characterized in that: this system also comprises flowmeter, and described flowmeter is arranged in the eluent export pipeline of each post bottom of array chromatographic column.
5. according to the continuous preparative chromatography of the described array of claim 1 system, it is characterized in that: described switch board also links to each other with feedstock pump, solvent pump respectively, and they are controlled.
6. according to the continuous preparative chromatography of the described array of claim 1 system, it is characterized in that: described feedstock pump and solvent pump are volume pumps.
7. according to the optional continuous preparative chromatography of described array system among the claim 1-6, it is characterized in that: described flow control valve is a hand valve.
8. according to the optional continuous preparative chromatography of described array system among the claim 1-6, it is characterized in that: described flow control valve is a motorized valve, described flowmeter is the flowmeter of belt sensor, this flowmeter is connected with switch board respectively with flow control valve, by the computer control piping flow.
9. the using method of the continuous preparative chromatography of array system, it is characterized in that: when solvent is sent into each post of array chromatographic column continuously equably, divide a valve to control to each charging control, with the feeding manner of simulation circular chromatography switch successively ground, periodically, equably to each the post charging of array chromatographic column.
10. using method according to claim 9 is characterized in that: described control method to each charging control branch valve is by establishing array chromatogram control program software in the computing machine, dividing valve to control by switch board to each charging control.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101294975B (en) * | 2008-06-19 | 2013-06-05 | 中国科学院生态环境研究中心 | Grouping toxicology analyzer |
| CN104655768A (en) * | 2015-03-11 | 2015-05-27 | 天津博纳艾杰尔科技有限公司 | Automatic crude oil component separating device and application of automatic crude oil component separating device in separation wax and colloid in crude oil |
| CN107142337A (en) * | 2017-05-19 | 2017-09-08 | 南京凯通粮食生化研究设计有限公司 | A kind of method that xylose and arabinose are prepared by raw material of bagasse |
| CN107615058A (en) * | 2015-06-01 | 2018-01-19 | 株式会社岛津制作所 | Preparative chromatograph |
| CN113493429A (en) * | 2021-05-22 | 2021-10-12 | 山东兆光色谱分离技术有限公司 | Industrialized gulonic acid three-component separation system and separation method thereof |
| US11389787B2 (en) | 2019-02-20 | 2022-07-19 | Kara Technologies Inc. | Catalyst structure and method of upgrading hydrocarbons in the presence of the catalyst structure |
| CN115078558A (en) * | 2021-03-16 | 2022-09-20 | 株式会社岛津制作所 | Preparative liquid chromatograph and analysis method |
| US11725150B2 (en) | 2020-08-18 | 2023-08-15 | Kara Technologies Inc. | Method of light oil desulfurization in the presence of methane containing gas environment and catalyst structure |
| US12006475B2 (en) | 2020-08-26 | 2024-06-11 | Kara Technologies Inc. | Organic solid biomass conversion for liquid fuels/chemicals production in the presence of methane containing gas environment and catalyst structure |
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2003
- 2003-09-19 CN CN 03146864 patent/CN1283993C/en not_active Expired - Fee Related
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101294975B (en) * | 2008-06-19 | 2013-06-05 | 中国科学院生态环境研究中心 | Grouping toxicology analyzer |
| CN104655768A (en) * | 2015-03-11 | 2015-05-27 | 天津博纳艾杰尔科技有限公司 | Automatic crude oil component separating device and application of automatic crude oil component separating device in separation wax and colloid in crude oil |
| CN104655768B (en) * | 2015-03-11 | 2016-08-17 | 天津博纳艾杰尔科技有限公司 | Oil component automatic separation equipment and the application in wax, colloid separation in crude oil thereof |
| CN107615058A (en) * | 2015-06-01 | 2018-01-19 | 株式会社岛津制作所 | Preparative chromatograph |
| CN107615058B (en) * | 2015-06-01 | 2020-01-17 | 株式会社岛津制作所 | Preparative chromatograph |
| CN107142337A (en) * | 2017-05-19 | 2017-09-08 | 南京凯通粮食生化研究设计有限公司 | A kind of method that xylose and arabinose are prepared by raw material of bagasse |
| US11833492B2 (en) | 2019-02-20 | 2023-12-05 | Kara Technologies, Inc. | Catalyst structure and method of upgrading hydrocarbons in the presence of the catalyst structure |
| US11389787B2 (en) | 2019-02-20 | 2022-07-19 | Kara Technologies Inc. | Catalyst structure and method of upgrading hydrocarbons in the presence of the catalyst structure |
| US11725150B2 (en) | 2020-08-18 | 2023-08-15 | Kara Technologies Inc. | Method of light oil desulfurization in the presence of methane containing gas environment and catalyst structure |
| US12006475B2 (en) | 2020-08-26 | 2024-06-11 | Kara Technologies Inc. | Organic solid biomass conversion for liquid fuels/chemicals production in the presence of methane containing gas environment and catalyst structure |
| CN115078558A (en) * | 2021-03-16 | 2022-09-20 | 株式会社岛津制作所 | Preparative liquid chromatograph and analysis method |
| CN113493429A (en) * | 2021-05-22 | 2021-10-12 | 山东兆光色谱分离技术有限公司 | Industrialized gulonic acid three-component separation system and separation method thereof |
| CN113493429B (en) * | 2021-05-22 | 2022-10-21 | 山东兆光色谱分离技术有限公司 | Industrialized gulonic acid three-component separation device and separation method thereof |
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