CN107413072B - Modularized multi-stage chromatographic column and sampling and separating method thereof - Google Patents
Modularized multi-stage chromatographic column and sampling and separating method thereof Download PDFInfo
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- CN107413072B CN107413072B CN201710734224.9A CN201710734224A CN107413072B CN 107413072 B CN107413072 B CN 107413072B CN 201710734224 A CN201710734224 A CN 201710734224A CN 107413072 B CN107413072 B CN 107413072B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/18—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns
- B01D15/1864—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns using two or more columns
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
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Abstract
The invention provides a modularized multi-stage chromatographic column and a sampling and separating method thereof. Compared with the prior art, the invention has the beneficial effects that: in the separation and purification process, the inside of the column can be sampled in real time so as to monitor the separation condition of the chromatographic column and realize dynamic monitoring; the number of the columns can be increased or reduced flexibly according to the requirement; when different components are separated in the column body, the column body with different components can be separated and respectively combined with the column top and the column bottom to be assembled into a plurality of chromatographic columns for use; the method has the characteristics of strong practicability, high flexibility and wide application range.
Description
Technical Field
The invention relates to a modularized multi-stage chromatographic column and a sampling and separating method thereof, which can sample and analyze liquid in the column in real time and can be separated and freely combined.
Background
At present, in an organic chemical synthesis laboratory, a chromatographic column is commonly used, wherein a column top, a column body and a column bottom are integrated, cannot be separated, and cannot sample and analyze liquid in the column body; the column height is fixed and the specification is various. In the using process of the chromatographic columns, in the separation and purification process, the components in the columns cannot be sampled and analyzed, and only whether the pure compounds are separated or not can be obtained through sampling and analysis of the liquid outlet at the bottom of the column, the separation process is full of uncertainty, and the separation and purification process is not feasible for the unseparated pure mixed components, only the separation and purification process can be carried out again, a large amount of resources and labor cost are wasted, and the separation and purification efficiency is greatly influenced; when two compound components with large polarity difference are separated, the undeployed upper component cannot be eluted immediately when the components with small polarity are separated, a large amount of eluent is needed to be used for leading the upper component to run to the whole column height, the components are separated from a liquid outlet, a large amount of eluent is consumed, and the method is not economical and environment-friendly; when separating compounds with similar polarity, particularly isomers, the separation is difficult, the column height is increased and is limited by the column height, the higher column is customized, a great deal of cost is consumed, the utilization rate is low, the operation difficulty is high and the operation site is limited. The defects determine that the current chromatographic column cannot be economical, environment-friendly, energy-saving and efficient, and is not suitable for the current increasingly complex separation system.
As the demand for chromatographic separations continues to increase, so too does the development of chromatographic columns, for example: for flexible setting of the heights of the separation process chromatography column and the adsorbent, CN201320200721.8 discloses a combined chromatography column, but it can only be used by freely configuring the number of columns before the separation and purification operation; in order to save the amount of eluent and increase the yield of samples, CN201521102771.8 discloses a combined chromatographic separation column, but it does not solve how to more effectively determine whether to separate pure compounds in a separation column before the column separation process; in order to realize column separation and separate elution, CN201420693338.5 discloses a split type multi-section chromatographic column, but it cannot accurately detect whether components in the column are separated into different column sections, and it is difficult to overcome huge vacuum pressure in the separation and purification process to separate the chromatographic column filled with liquid, and when the products are eluted separately, the packing in the single-stage column needs to be taken out, and the operation steps are increased. The comprehensive analysis has no good scheme, can timely detect the separation condition of the chromatographic column in the separation and purification process of the chromatographic column, and can perform column separation according to detection and analysis results to perform elution or increase or decrease the number of columns to continue purification and separation.
Therefore, to meet the requirements of sampling and column separation in chromatographic separation of compounds, it is necessary to design a new analytical separation scheme.
Disclosure of Invention
Aiming at the problems existing in the background technology, the invention provides the chromatographic column with strong practicability, high flexibility, strong operability and wide application range.
The invention is realized in the following way: the modular multistage chromatographic column comprises a column top, at least one section of column body and a column bottom which are nested in sequence from top to bottom, wherein nested surfaces of the column top, the column body and the column bottom, which are mutually matched, are frosted surfaces, a sample inlet is arranged on the column top, a liquid outlet is arranged below the column body, a control valve is arranged on the liquid outlet, a column top sampling small hole is penetrated through the nested surface of the column top, an upper sampling small hole is penetrated through the nested surface of the upper end of the column body, a lower sampling small hole is penetrated through the nested surface of the lower end of the column body, a sand core is arranged above the lower sampling small hole, a column bottom sampling small hole is penetrated through the nested surface of the column bottom, the column top sampling small hole and the upper sampling small hole can be communicated or not communicated through the relative position of the column top and the column body, the lower sampling small hole of the upper section of the column body and the upper sampling small hole of the lower section of the column body can be communicated or not communicated through the relative position of the rotary column body, and the lower sampling small hole of the column bottom can be communicated or not communicated through the relative position of the rotary column bottom and the column bottom sampling small hole.
Vacuum silicone grease is smeared between the frosting surfaces of the nested parts.
The apertures of the column top sampling small hole, the upper sampling small hole, the lower sampling small hole and the column bottom sampling small hole are the same.
The diameter of the sand core is matched with the inner diameter of the cylinder.
And the sample inlet is detachably connected with a grinding plug.
The sampling method of the modularized multi-stage chromatographic column is divided into normal pressure sampling in the column and negative pressure sampling in the column; the normal pressure sampling in the column aligns the lower sampling small hole of the upper section column with the upper sampling small hole of the lower section column by rotating the relative positions of the upper section column and the lower section column at the nesting position, and the liquid in the column flows out due to pressure intensity to sample; the negative pressure sampling is carried out in the column, a corresponding grinding plug is added at the upper nested part of the top of the column before sampling, then the solvent at the liquid outlet of the bottom of the column continuously flows out, when the liquid at the liquid outlet of the bottom of the column slowly drops, the control valve at the bottom of the column is closed, the upper column and the lower column are rotated, the solvent outflow rate at the position of the sampling small hole is slowed down under the combined action of the cavity negative pressure above the solvent and the atmospheric pressure outside the sampling small hole, and the trace solvent flowing out of the sampling small hole can be sampled.
The separation method of the modularized multistage chromatographic column comprises the steps of adding a sealed grinding plug on the top of the column before separating the column, simultaneously enabling solvent at a liquid outlet to continuously flow out to completely stop, closing a control valve at the bottom of the column, communicating the sampling small hole of each stage with the atmosphere, enabling air at the sampling small hole to enter a nested position below a sand core, separating the whole part above the sampling small hole, and enabling the solvent above the sand core not to flow out due to the surface tension at the sand core and the negative pressure above the liquid, so that the column can be freely separated or combined.
Compared with the prior art, the invention has the beneficial effects that: dynamically monitoring the condition of separating substances by solvent in the column, and freely separating and combining the columns to assemble a plurality of chromatographic columns, and increasing and decreasing the column height; under the condition of not affecting common pressurization and decompression separation, the device has the advantages of strong practicability, high flexibility, strong operability and wide application range, and can meet the increasingly complex and diversified organic matter separation requirements.
Drawings
FIG. 1 is a schematic structural view of a column top;
FIG. 2 is a schematic structural view of a column;
FIG. 3 is a schematic view of the structure of the column bottom;
FIG. 4 is a schematic structural view of a modular multi-stage chromatography column comprising three sections of chromatography columns and a method for sampling and separating the same;
FIG. 5 is a schematic view of the structure of FIG. 4 in which the sampling holes at section E are not in communication;
fig. 6 is a schematic view of the structure of fig. 4 in which the sampling holes at section E are in communication.
The device comprises a 1-column top, a 2-column, a 3-column bottom, a 4-sample inlet, a 5-liquid outlet, a 6-control valve, a 7-column top sampling pore, an 8-upper sampling pore, a 9-lower sampling pore, a 10-column bottom sampling pore and an 11-sand core.
Detailed description of the preferred embodiments
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent.
Aiming at the problems existing in the background technology, the invention provides the chromatographic column with strong practicability, high flexibility, strong operability and wide application range, and provides a dynamic monitoring scheme for sampling and analyzing components in the column and a scheme for separating and freely assembling the column in the chromatographic separation process.
The drawings include the following components: the column top 1, the column body 2, the column bottom 3, the sample inlet 4, the liquid outlet 5, the control valve 6, the column top sampling small hole 7, the upper sampling small hole 8, the lower sampling small hole 9, the column bottom sampling small hole 10 and the sand core 11.
As shown in figures 1-6, the modularized multi-stage chromatographic column and the sampling and separating method thereof comprise a column top, at least one section of column body and a column bottom which are nested from top to bottom in sequence, wherein nested surfaces of the column top, the column body and the column bottom are mutually matched, the column top is provided with a sample inlet, a liquid outlet is arranged below the column, a control valve is arranged on the liquid outlet, a column top sampling small hole is penetrated through the nested surface of the column top, an upper sampling small hole is penetrated through the nested surface of the upper end of the column body, a lower sampling small hole is penetrated through the nested surface of the lower end of the column body, a sand core is arranged above the lower sampling small hole of the column body, a column bottom sampling small hole is penetrated through the nested surface of the column bottom, the lower sampling small hole of the column top and the upper sampling small hole of the column body can be communicated or not communicated through the relative position of the rotary column top and the upper sampling small hole of the column body, and the lower sampling small hole of the upper section of the column body can be communicated or not communicated through the relative position of the rotary column body and the lower sampling small hole of the column bottom.
Vacuum silicone grease is smeared between the frosting surfaces of the nested parts.
The apertures of the column top sampling small hole, the upper sampling small hole, the lower sampling small hole and the column bottom sampling small hole are the same.
The diameter of the sand core is matched with the inner diameter of the cylinder.
And the sample inlet is detachably connected with a grinding plug.
The sampling method of the modularized multi-stage chromatographic column is divided into normal pressure sampling in the column and negative pressure sampling in the column; the normal pressure sampling in the column aligns the lower sampling small hole of the upper section column with the upper sampling small hole of the lower section column by rotating the relative positions of the upper section column and the lower section column at the nesting position, and the liquid in the column flows out due to pressure intensity to sample; the negative pressure sampling is carried out in the column, a corresponding grinding plug is added at the upper nested part of the top of the column before sampling, then the solvent at the liquid outlet of the bottom of the column continuously flows out, when the liquid at the liquid outlet of the bottom of the column slowly drops, the control valve at the bottom of the column is closed, the upper column and the lower column are rotated, the solvent outflow rate at the position of the sampling small hole is slowed down under the combined action of the cavity negative pressure above the solvent and the atmospheric pressure outside the sampling small hole, and the trace solvent flowing out of the sampling small hole can be sampled.
The separation method of the modularized multistage chromatographic column comprises the steps of adding a sealed grinding plug on the top of the column before separating the column, simultaneously enabling solvent at a liquid outlet to continuously flow out to completely stop, closing a control valve at the bottom of the column, communicating the sampling small hole of each stage with the atmosphere, enabling air at the sampling small hole to enter a nested position below a sand core, separating the whole part above the sampling small hole, and enabling the solvent above the sand core not to flow out due to the surface tension at the sand core and the negative pressure above the liquid, so that the column can be freely separated or combined.
Examples
Each section of column body can be independently assembled with the column top and the column bottom to form a chromatographic column, or the multi-section column body can be combined with the column top and the column bottom for use; the position of a sampling small hole at the nesting position of the adjacent columns can be adjusted in the use process, sampling analysis is carried out, dynamic detection is realized, and according to the requirement of the sampling process, in-column normal pressure sampling with little loss of solvent and in-column negative pressure sampling with little loss of solvent can be carried out; in the separation and purification process, the separation columns can be respectively assembled into new chromatographic columns for elution and separation respectively; the number of the columns without components above can be reduced, the number of the columns with separating materials filled below can be increased, and the problems in the separation and purification process can be flexibly solved.
Example 1: dynamic monitoring-in-column normal pressure sampling
The normal pressure sampling in the column uses the principle of liquid pressure, and the lower sampling small hole of the upper column body is aligned with the upper sampling small hole of the lower column body by rotating the relative positions of the upper column body and the lower column body at the nesting position, so that the liquid in the column flows out due to the pressure, the sampling is performed, the solvent loss is reduced, the rapid rotation is needed, and the time for the two sampling small holes to be right facing each other is reduced.
As shown in FIG. 4, a three-stage chromatographic column is exemplified by a combination of 3 sections of columns, and a section of a nesting position of the 2 nd section of column and the 3 rd section of column is shown in FIG. 5. The embodiment comprises the following steps: the column top 1,3 sections of column bodies 2 and column bottom 3 are sleeved with the nested surfaces through frosting treatment to ensure tightness, and lubricant such as vacuum silicone grease is smeared between the nested surfaces, so that the vacuum silicone grease can ensure air tightness and can ensure free relative rotation between the modules without influencing separation.
As shown in fig. 5 and 6, the separation condition of the section 2 column is sampled and analyzed, the section 3 column and below is directly fixed, the section 2 column and above are rotated to enable the lower sampling small hole 9 of the section 2 column to be opposite to the upper sampling small hole 8 of the section 3 column, at this time, the column is communicated with the atmosphere at the sampling small hole, and the solvent in the column flows out of the sampling small hole under the action of the liquid pressure, so that the solvent can be sampled.
In order to reduce the solvent loss of chromatographic separation by sampling, the two sampling pores need to be rotated rapidly to shorten the facing time.
Example 2: dynamic monitoring-in-column negative pressure sampling
The method comprises the steps of sampling the negative pressure in the column, adding a corresponding grinding plug at the upper nested part of the top of the column before sampling, sealing, enabling solvent at the liquid outlet of the bottom of the column to continuously flow out, generating negative pressure in a cavity above the solvent in the chromatographic column at the moment, closing a control valve at the bottom of the column when liquid at the liquid outlet of the bottom of the column slowly drops, and at the moment, enabling the pressure generated by the negative pressure in the cavity above the solvent to balance most of solvent gravity.
Before sampling, a grinding plug is added at the sample inlet 4 of the column top 1 to realize the sealing of the column, the solvent in the column continuously flows out, the negative pressure is generated in the upper cavity of the 1 st column solvent due to the reduction of the solvent, when the solvent is slowly dropped out from the liquid outlet 5 of the column bottom 3, the pressure generated by the negative pressure in the cavity above the solvent counteracts most of the gravity of the solvent, at the moment, the sampling operation is repeated, the solvent outflow quantity at the small sampling hole can be obviously reduced, and the purpose of controlling the solvent loss is achieved.
According to the operation, the sampling analysis can be carried out on each sampling small hole of the multi-section chromatographic column body so as to achieve the purpose of dynamic monitoring.
Example 3: free combination-column separation
Before the column body is separated, a sealed grinding plug is added on the top of the column, and simultaneously, the solvent at a liquid outlet continuously flows out to be completely stopped, namely, the complete negative pressure can be formed above the liquid in the column, the pressure difference generated by the negative pressure in the column is balanced with the gravity of the liquid in the whole chromatographic column, at the moment, a control valve at the bottom of the column is closed, when the sampling small hole of each stage is communicated with the atmosphere, the pressure difference formed at the sampling small hole is greater than the gravity of the liquid above the sampling small hole, at the moment, air enters the nesting position below a sand core, the part above the sampling small hole can be integrally separated, and the solvent above the sand core can not flow out due to the surface tension at the sand core and the negative pressure effect above the liquid, so that the free separation combination of the chromatographic column can be realized, the free separation and the respective elution can be realized, the flexible operations such as the increase and the column height can be realized.
Taking the nesting position of the section 2 column body and the section 3 column body as an example, separating the two column bodies, referring to the negative pressure sampling operation, under the same conditions, adding a grinding plug at the sample inlet of the column top 1 to realize the sealing of the column bodies, continuously flowing out the solvent in the column bodies to a complete stop, balancing the pressure generated by the negative pressure generated by the cavity above the solvent with the gravity of the solvent, rotating the upper part of the section 3 column bodies at the moment, leading the sampling small holes to be opposite and communicated with the atmosphere, and because the negative pressure generated by the cavity in the column bodies is balanced with the solvent in the whole chromatographic column, the pressure generated by the negative pressure is greater than the gravity of the solvent above the sampling small holes, the air enters the position below a sand core inside the column bodies, and the solvent above the sand core can not continuously flow out, thus the section 2 column bodies and the section 3 column bodies can be separated.
Dividing the three-stage chromatographic column into an upper part and a lower part, combining the original column top, the 1 st and 2 nd sections of columns and 1 new column bottom to form a new chromatographic column, and combining the 1 new column top, the 3 rd section of columns and the original column bottom to form another new chromatographic column; one or more sections of columns filled with filler and solvent can be added between the separated column 3 and the column bottom according to the requirement, and the columns are assembled for continuous chromatographic separation. Thus, the purposes of separation and free combination of the chromatographic column bodies can be achieved.
The foregoing description of the preferred embodiment of the invention is not intended to be limiting, but rather to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (7)
1. The utility model provides a multistage chromatographic column of modularization, includes from top to bottom nested post top in proper order, at least one section cylinder and post end, and the nested face of mutually supporting of nested department between post top, cylinder and the post end is the frosting, is equipped with the inlet on the post top, is equipped with the liquid outlet below the post, is equipped with the control valve on the liquid outlet, its characterized in that: a column top sampling small hole is communicated with the nesting surface of the column top, an upper sampling small hole is communicated with the nesting surface of the upper end of the column body, a lower sampling small hole is communicated with the nesting surface of the lower end of the column body, a sand core is arranged above the lower sampling small hole of the column body, a column bottom sampling small hole is communicated with the nesting surface of the column bottom, the column top sampling small hole and the upper sampling small hole can be communicated or not communicated with each other through the relative position of the rotary column top and the column body, the lower sampling small hole of the upper section of column body and the upper sampling small hole of the lower section of column body are communicated or not communicated through the relative position of the rotary column body and the column bottom sampling small hole, and the lower sampling small hole and the column bottom sampling small hole can be communicated or not communicated through the relative position of the rotary column body and the column bottom.
2. The modular multi-stage chromatography column of claim 1, wherein: vacuum silicone grease is smeared between the frosting surfaces of the nested parts.
3. The modular multi-stage chromatography column of claim 1, wherein: the apertures of the column top sampling small hole, the upper sampling small hole, the lower sampling small hole and the column bottom sampling small hole are the same.
4. The modular multi-stage chromatography column of claim 1, wherein: the diameter of the sand core is matched with the inner diameter of the cylinder.
5. The modular multi-stage chromatography column of claim 1, wherein: and the sample inlet is detachably connected with a grinding plug.
6. The method for sampling a modular multi-stage chromatography column according to claim 1, wherein: the method is divided into in-column normal pressure sampling and in-column negative pressure sampling; the normal pressure sampling in the column aligns the lower sampling small hole of the upper section column with the upper sampling small hole of the lower section column by rotating the relative positions of the upper section column and the lower section column at the nesting position, and the liquid in the column flows out due to pressure intensity to sample; the negative pressure sampling is carried out in the column, a corresponding grinding plug is added at the upper nested part of the top of the column before sampling, then the solvent at the liquid outlet of the bottom of the column continuously flows out, when the liquid at the liquid outlet of the bottom of the column slowly drops, the control valve at the bottom of the column is closed, the upper column and the lower column are rotated, the solvent outflow rate at the position of the sampling small hole is slowed down under the combined action of the cavity negative pressure above the solvent and the atmospheric pressure outside the sampling small hole, and the trace solvent flowing out of the sampling small hole can be sampled.
7. The method of separating a modular multi-stage chromatography column of claim 1, wherein: before the cylinder is separated, a sealed grinding plug is added on the top of the cylinder, and simultaneously, the solvent at the liquid outlet is continuously flowed out to be completely stopped, at the moment, a control valve at the bottom of the cylinder is closed, the sampling small hole of each stage is communicated with the atmosphere, at the moment, air enters the nesting position below the sand core at the sampling small hole, the part above the sampling small hole can be wholly separated, the solvent above the sand core can not flow out due to the surface tension at the sand core and the negative pressure above the liquid, and the cylinder can be freely separated or combined.
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| CN108165759A (en) * | 2018-01-30 | 2018-06-15 | 芒市海华开发有限公司 | A kind of combined type desorption column |
| CN114072216B (en) * | 2019-06-28 | 2023-07-07 | 夏尔巴生物技术(苏州)有限公司 | Modular chromatography device |
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| US20020185442A1 (en) * | 1998-10-30 | 2002-12-12 | Maiefski Romaine R. | Sample separation apparatus and method for multiple channel high throughput purification |
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