CN106731001B - Split type countercurrent chromatographic separation column - Google Patents
Split type countercurrent chromatographic separation column Download PDFInfo
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- CN106731001B CN106731001B CN201710004737.4A CN201710004737A CN106731001B CN 106731001 B CN106731001 B CN 106731001B CN 201710004737 A CN201710004737 A CN 201710004737A CN 106731001 B CN106731001 B CN 106731001B
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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
- B01D15/1807—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns using counter-currents, e.g. fluidised beds
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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
- B01D15/22—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the construction of the column
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Abstract
The invention discloses a split type countercurrent chromatographic separation column, which comprises two separation columns I and II of a semi-cylindrical structure integrally formed by a 3D printing technology, wherein a reticular sealing gasket is arranged between the two separation columns of the semi-cylindrical structure to seal the two separation columns, the side walls of the two separation columns of the semi-cylindrical structure are connected into a whole through a connecting device, and the central line of a mounting hole of the connecting device is vertical to the axes of the two separation columns; a certain pressure is applied to the net-shaped sealing gasket by the fastening of the connecting device. The invention changes the closed structure of the traditional separation column pipeline into two open units, changes the cleaning of one pipeline into the cleaning of a plurality of open pipelines, and is easy to clean powder in the pipelines.
Description
Technical Field
The invention relates to the field of separation and analysis instruments, in particular to a split type 3D printed countercurrent chromatographic separation column.
Background
The high-speed counter-current chromatography is based on liquid-liquid partition chromatography, and is characterized in that immiscible two phase solvents are continuously mixed to repeatedly partition a sample, and the sample is sequentially eluted according to a partition coefficient. Because no solid carrier or support is needed, the high-efficiency separation and preparation can be realized in a short time, and thousands of theoretical plates can be reached. Compared with other separation chromatographs, the method overcomes the defects of sample adsorption, loss, pollution and the like caused by a stationary phase carrier, and has the advantages of low cost, recoverable solvent and the like.
The countercurrent chromatographic separation column is the core of countercurrent chromatography, the conventional countercurrent chromatographic separation column is composed of a polytetrafluoroethylene tube and a pipeline support body, the polytetrafluoroethylene tube is wound on the pipeline support body in a multilayer mode, the countercurrent chromatographic separation column with the structure is limited by a commercialized polytetrafluoroethylene tube, innovation on the pipeline structure is difficult to carry out, and the function development of the countercurrent chromatographic column is limited.
The 3D printing technology is also called additive manufacturing technology, is different from the traditional manufacturing method of die making processing, realizes layer-by-layer processing and overlapping forming through a machine, gets rid of the constraint of space geometry and design process, can convert any creative design into an entity product, and expands huge creative space. The technology overcomes the defect that the traditional countercurrent chromatographic separation column is limited by a commercial polytetrafluoroethylene tube, and can be innovated on the tube type of the separation column. Considering that organic solvents are generally used in countercurrent chromatography separation two-phase solvent systems, metal powders resistant to corrosion by organic solvents are the material of choice for 3D printing. However, the 3D printing process of the metal powder material is limited by the layer-by-layer powder laying process, the specific gravity of the metal powder material is too high, and the cleaning of powder in a long pipeline after printing is difficult. Therefore, the structure of the split type countercurrent chromatographic separation column needs to be innovated, and the metal powder in the pipeline can be completely cleaned.
Disclosure of Invention
The invention provides a split type countercurrent chromatographic separation column aiming at the technical difficulty in a 3D printing countercurrent chromatographic separation column made of metal powder.
The technical scheme adopted by the invention is as follows:
a split type countercurrent chromatographic separation column comprises two separation columns I and II which are integrally formed by a 3D printing technology and have a semi-cylindrical structure, wherein a reticular sealing gasket is arranged between the two separation columns with the semi-cylindrical structure to seal the two separation columns, the side walls of the two separation columns with the semi-cylindrical structure are connected into a whole through a connecting device, and the central line of a mounting hole of the connecting device is vertical to the axes of the two separation columns; and certain pressure is applied to the net-shaped sealing gasket through fastening of the connecting device, so that the sealing performance of the whole device is ensured.
Furthermore, the external structures of the separation columns of the two semi-columnar structures are completely the same; the two semi-columnar separation columns and the reticular sealing gasket are combined together to form a cylindrical separation column.
Further, the separation columns of the two semi-columnar structures and the inside of the meshed sealing gasket are provided with cylindrical holes for transmitting samples, after the three components are combined, a plurality of circles of cylindrical holes which are communicated end to end are formed between all the cylindrical holes, one end of each cylindrical hole is a sample inlet, and the other end of each cylindrical hole is a sample outlet.
The connection mode of the separation columns of the two semi-columnar structures is as follows:
furthermore, the connecting device is a screw, corresponding screw mounting holes are formed in the side walls of the two separation columns with the semi-columnar structures and the upper part and the lower part of the reticular sealing gasket, and the positions of the screw mounting holes in the upper parts are higher than the position of the cylindrical hole at the highest point; the screw mounting hole at the lower part is lower than the cylindrical hole at the lowest point.
The screw mounting holes of the separation column with the semi-columnar structure and the reticular sealing gasket are through holes; the screw mounting hole of the separation column of the other semi-columnar structure is a blind hole, the blind hole and the axis of the through hole are in the same straight line, and screws are mounted in the blind hole and the through hole.
And the second connection mode of the separation columns of the two semi-columnar structures is as follows:
further, the connecting device is a screw, corresponding screw mounting holes are formed in the upper portion and the lower portion of the side wall of each of the two separation columns with the semi-columnar structures, and the positions of the screw mounting holes in the upper portions are higher than the position of the columnar hole at the highest point; the position of the screw mounting hole at the lower part is lower than the position of the cylindrical hole at the lowest point.
The screw mounting hole of one of the semi-columnar separation columns is a through hole; the screw mounting hole of the separation column of the other semi-columnar structure is a blind hole, the blind hole and the axis of the through hole are in the same straight line, and screws are mounted in the blind hole and the through hole.
Furthermore, in the two connection modes, the screw mounting holes comprise a plurality of screw mounting holes which are distributed along the circumferential direction of the side wall of the separation column of the semi-columnar structure, and the center lines of the screw mounting holes positioned at the upper part are positioned on the same horizontal plane; the central lines of the plurality of screw mounting holes positioned at the lower part are positioned on the same horizontal plane.
Furthermore, the material of the reticular sealing gasket is a corrosion-resistant material which can resist pressure and ensure the sealing property, such as polytetrafluoroethylene material, polytetrafluoroethylene material and the like.
The invention has the following beneficial effects:
1. the closed structure of the traditional separation column pipeline is changed into two open units, the cleaning of one pipeline is changed into the cleaning of a plurality of open pipelines, and the powder in the pipelines is easy to clean;
2. the corrosion-resistant mesh gasket has the advantages of organic solvent corrosion resistance, material compression and good sealing performance;
3. the design of the tensioning screw ensures that the tetrafluoroethylene mesh gasket is uniformly stressed after being extruded, and the separation column does not leak liquid.
4. The tensioning screw is arranged in the whole separation column, so that the whole volume of the separation column is not increased, and the miniaturization of the separation column can be further realized.
5. According to the invention, the screw mounting holes are arranged in the whole separation column, so that the connection of the separation column is realized, the whole volume of the separation column is not increased, the separation column can be well matched with the existing equipment, and the cost is further saved.
Drawings
In order to more clearly illustrate the embodiments or technical solutions of the present invention, the drawings used in the embodiments or technical solutions in the prior art are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a top view of a split counter-current chromatographic separation column;
FIG. 2 is a schematic cross-sectional view of a split countercurrent chromatography separation column;
FIG. 3 is a schematic cross-sectional view of a split countercurrent chromatography separation column;
FIG. 4 is a schematic view of a mesh pad of a split countercurrent chromatography separation column;
FIG. 5 is a schematic diagram of a three-dimensional overall structure of a split countercurrent chromatography separation column;
in the figure: 1-separation column splitting; 2-a reticular sealing gasket; 3-separating column splitting; 4-tightening the screw.
Detailed Description
The invention is described in detail below with reference to the accompanying drawings:
the invention provides a split type countercurrent chromatography separation column aiming at the problem that metal powder materials of the existing split type countercurrent chromatography separation column are difficult to clean, and as shown in figures 1, 2, 3 and 5, the split type countercurrent chromatography separation column printed by 3D comprises two separation columns which are integrally formed by 3D printing technology and have semi-columnar structures, namely a separation column split body 1 and a separation column split body 3, the side walls of the separation column split body 1 and the separation column split body 3 are connected into a whole through screws, the screws sequentially penetrate through the separation column 1, a reticular sealing gasket 2 and the separation column 3, and the central line of mounting holes of the screws is vertical to the axes of the two separation columns; a certain pressure is applied to the mesh-like sealing gasket by tightening the screw, which does not pass through the separation column 3.
The invention changes the closed structure of the traditional separation column pipeline into two open units, changes the cleaning of one pipeline into the cleaning of a plurality of open pipelines, and is easy to clean powder in the pipelines;
furthermore, the appearance structure of the separation column split 1 is completely the same as that of the separation column split 3; the two semi-columnar separation columns and the reticular sealing gasket are combined together to form a cylindrical separation column.
Further, the separation column components of a whole that can function independently 1, 3 and the netted sealed pad 2 inside of two semi-columnar structures all be equipped with and be used for transmitting sample cylindricality hole, and three part combination backs, form the many rings of cylindricality hole of head and the tail intercommunication between all cylindricality holes, the one end in cylindricality hole is the sample entry, and the separation column import promptly, the other end is the sample export, separation column export promptly.
The connection between the separation column split body 1 and the separation column split body 3 is performed in two ways:
the first method is as follows:
corresponding screw mounting holes are formed in the side walls of the separation column split bodies 1 and 3 of the two semi-columnar structures and the upper part and the lower part of the reticular sealing gasket 2, and the positions of the screw mounting holes in the upper parts are higher than the position of a cylindrical hole at the highest point; the position of the screw mounting hole at the lower part is lower than the position of the cylindrical hole at the lowest point.
As shown in fig. 2, the screw mounting holes of the separation column split body 1 and the reticular sealing gasket 2 of one semi-columnar structure are through holes; the screw mounting hole of the separation column split body 3 with the other semi-columnar structure is a blind hole, the blind hole and the axis of the through hole are in the same line, and screws are mounted in the blind hole and the through hole.
And threads matched with the screws are arranged in the blind holes and the through holes.
The screw mounting holes comprise a plurality of screws, one screw mounting hole is used for mounting one screw, the screws are sequentially distributed along the circumferential direction of the side wall of the separation column of the semi-columnar structure, and the central lines of the screw mounting holes positioned at the upper part are positioned on the same horizontal plane; the central lines of the plurality of screw mounting holes positioned at the lower part are positioned on the same horizontal plane.
The second method comprises the following steps:
corresponding screw mounting holes are only arranged at the upper part and the lower part of the side walls of the separation column split bodies 1 and 3 with the two semi-columnar structures, and the positions of the screw mounting holes at the upper parts are higher than the position of a columnar hole at the highest point; the position of the screw mounting hole at the lower part is lower than the position of the cylindrical hole at the lowest point.
The screw mounting hole of the separation column split body 1 of one semi-columnar structure is a through hole; the screw mounting hole of the separation column split 3 of the other semi-column structure is a blind hole, the blind hole and the axis of the through hole are in the same straight line, and screws are mounted in the blind hole and the through hole. And threads matched with the screws are arranged in the blind holes and the through holes.
The screw mounting holes comprise a plurality of screws, one screw is mounted in each screw mounting hole, the screws are sequentially distributed along the circumferential direction of the side wall of the separation column of the semi-columnar structure, and the central lines of the screw mounting holes positioned at the upper part are positioned on the same horizontal plane; the central lines of a plurality of screw mounting holes positioned at the lower part are positioned on the same horizontal plane.
The two modes can be different from the gasket, the screw mounting holes are arranged in the whole separation column, the connection of the separation column is realized, the integral volume of the separation column is not increased, the separation column can be well matched with the existing equipment, and the cost is further saved.
Meanwhile, the design of the tensioning screw ensures that the tetrafluoroethylene mesh gasket is uniformly stressed after being extruded, and the separation column is ensured not to leak liquid.
In example 2, the gasket structure is shown in fig. 4, and the material of the mesh-shaped sealing gasket is a corrosion-resistant material capable of withstanding pressure and ensuring sealing performance, such as polytetrafluoroethylene material and polytetrafluoroethylene material; the upper and lower portions of the net-shaped sealing gasket 2 are not provided with through holes for screws to pass through.
The screw in the invention can be designed into a bolt and replaced by the bolt, and the internal thread of the specific mounting hole is adjusted according to different bolts.
By using the 3D printing technology, the shape of the cylindrical hole is not limited, the cylindrical hole can be designed into any special-shaped structure, and the separation efficiency of the countercurrent chromatography is greatly improved.
Although the embodiments of the present invention have been described with reference to the accompanying drawings, it is not intended to limit the scope of the present invention, and it should be understood by those skilled in the art that various modifications and variations can be made without inventive efforts by those skilled in the art based on the technical solution of the present invention.
Claims (7)
1. A split type countercurrent chromatography separation column is characterized by comprising two separation columns I and II which are integrally formed by a 3D printing technology and have a semi-cylindrical structure, wherein a reticular sealing gasket is arranged between the two separation columns with the semi-cylindrical structure to seal the two separation columns, the side walls of the two separation columns with the semi-cylindrical structure are connected into a whole through a connecting device, and the central line of a mounting hole of the connecting device is vertical to the axes of the two separation columns; applying a certain pressure on the reticular sealing gasket by fastening the connecting device, arranging cylindrical holes for transmitting samples in the separating columns of the two semi-cylindrical structures and the reticular sealing gasket, and forming a plurality of circles of cylindrical holes which are communicated end to end among all the cylindrical holes after the three components are combined, wherein one end of each cylindrical hole is a sample inlet, and the other end of each cylindrical hole is a sample outlet; the appearance structures of the two separating columns of the semi-cylindrical structures are completely the same; the two separation columns with the semi-cylindrical structures and the reticular sealing gasket are combined together to form a separation column with a cylindrical structure.
2. The split-type countercurrent chromatographic separation column according to claim 1, wherein the connecting means is a screw, corresponding screw mounting holes are respectively arranged on the side walls of the two separation columns with semi-cylindrical structures and the upper part and the lower part of the reticular sealing gasket, and the position of the screw mounting hole at the upper part is higher than the position of the cylindrical hole at the highest point; the screw mounting hole at the lower part is lower than the cylindrical hole at the lowest point.
3. The split countercurrent chromatographic separation column according to claim 2, wherein the screw mounting holes of one of the semi-cylindrical separation column and the net-shaped sealing gasket are through holes; the screw mounting hole of the separating column of the other semi-cylindrical structure is a blind hole, the blind hole and the axis of the through hole are in the same straight line, and screws are mounted in the blind hole and the through hole.
4. The split-type countercurrent chromatographic separation column according to claim 1, wherein the connecting means is a screw, corresponding screw mounting holes are provided at the upper and lower parts of the side walls of the two separation columns with semi-cylindrical structures, and the screw mounting hole at the upper part is higher than the position of the cylindrical hole at the highest point; the screw mounting hole at the lower part is lower than the cylindrical hole at the lowest point.
5. The split countercurrent chromatographic separation column according to claim 4, wherein the screw mounting hole of one of the semi-cylindrical separation columns is a through hole; the screw mounting hole of the separating column of the other semi-cylindrical structure is a blind hole, the blind hole and the axis of the through hole are in the same straight line, and screws are mounted in the blind hole and the through hole.
6. The split countercurrent chromatographic separation column according to claim 2 or 4, wherein the screw mounting holes comprise a plurality of screw mounting holes distributed along the circumferential direction of the side wall of the separation column with a semi-cylindrical structure, and the center lines of the screw mounting holes at the upper part are on the same horizontal plane; the central lines of the plurality of screw mounting holes positioned at the lower part are positioned on the same horizontal plane.
7. The split countercurrent chromatographic separation column of claim 1, wherein the mesh sealing gasket is corrosion resistant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710004737.4A CN106731001B (en) | 2017-01-04 | 2017-01-04 | Split type countercurrent chromatographic separation column |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710004737.4A CN106731001B (en) | 2017-01-04 | 2017-01-04 | Split type countercurrent chromatographic separation column |
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| CN106731001A CN106731001A (en) | 2017-05-31 |
| CN106731001B true CN106731001B (en) | 2023-04-07 |
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| CN201710004737.4A Active CN106731001B (en) | 2017-01-04 | 2017-01-04 | Split type countercurrent chromatographic separation column |
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| US3869409A (en) * | 1972-06-08 | 1975-03-04 | Natalya Karlovna Bebris | Process for preparing a wide-pore adsorbent for use in chromatography |
| DE2922689A1 (en) * | 1978-06-07 | 1979-12-13 | Magnussen Jun | PUMPING DEVICE |
| JPH08327621A (en) * | 1995-02-24 | 1996-12-13 | Uop Inc | Solid silica capillary tube column used in chromatography |
| CN104117226A (en) * | 2014-07-04 | 2014-10-29 | 大连大学 | Sectional type high-efficiency column-mounting column chromatography combination device capable of adjusting column temperature and freely splitting |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105771317B (en) * | 2016-03-10 | 2020-06-02 | 山东省分析测试中心 | Countercurrent chromatography separation column and chromatograph |
| CN205650038U (en) * | 2016-05-18 | 2016-10-19 | 绿菱电子材料（天津）有限公司 | Small -size gas purification device |
| WO2018022119A1 (en) * | 2016-07-29 | 2018-02-01 | Westinghouse Electric Company Llc | Tank closure cesium removal |
| CN206414800U (en) * | 2017-01-04 | 2017-08-18 | 山东省分析测试中心 | A kind of split type countercurrent chromatography separation column |
| CN107982961A (en) * | 2018-01-08 | 2018-05-04 | 湖南科众源创科技有限公司 | The full-automatic chromatographic column of movable beam type |
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2017
- 2017-01-04 CN CN201710004737.4A patent/CN106731001B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3869409A (en) * | 1972-06-08 | 1975-03-04 | Natalya Karlovna Bebris | Process for preparing a wide-pore adsorbent for use in chromatography |
| DE2922689A1 (en) * | 1978-06-07 | 1979-12-13 | Magnussen Jun | PUMPING DEVICE |
| JPH08327621A (en) * | 1995-02-24 | 1996-12-13 | Uop Inc | Solid silica capillary tube column used in chromatography |
| CN104117226A (en) * | 2014-07-04 | 2014-10-29 | 大连大学 | Sectional type high-efficiency column-mounting column chromatography combination device capable of adjusting column temperature and freely splitting |
Non-Patent Citations (1)
| Title |
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| 天然棕色棉色素的液相色谱分离;马明波;《纺织学报》;20120731;全文 * |
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