阅读说明：本技术 一种工业大麻中纯化大麻二酚的双级层析柱分离系统 (Double-stage chromatographic column separation system for purifying cannabidiol in industrial cannabis sativa ) 是由 陈昕 孙田 吴义务 梁小勇 孙科 徐坚 于 2021-09-02 设计创作，主要内容包括：本发明公开了一种工业大麻中纯化大麻二酚的双级层析柱分离系统,涉及层析分离技术领域,包括层析组件,所述层析组件包括一级层析柱和二级层析柱,所述一级层析柱和二级层析柱通过固定架固定连接,所述一级层析柱和二级层析柱的顶部均设置有加液口,所述一级层析柱和二级层析柱的底部均设置有三通阀,所述三通阀的外部均固定连接有引液管和排液管,所述层析组件的顶部设置有加料罐。本发明通过设置二级层析柱,并将一级层析柱的引液管引至二级层析柱中进行二级层析,而通过将二级层析后的溶液引入至蒸发罐中蒸发浓缩再引入至二级层析柱中循环层析,提高了层析分离效果,提高了大麻二酚的提取效率。(The invention discloses a double-stage chromatographic column separation system for purifying cannabidiol in industrial hemp, which relates to the technical field of chromatographic separation and comprises a chromatographic assembly, wherein the chromatographic assembly comprises a primary chromatographic column and a secondary chromatographic column, the primary chromatographic column and the secondary chromatographic column are fixedly connected through a fixing frame, liquid adding ports are respectively arranged at the tops of the primary chromatographic column and the secondary chromatographic column, three-way valves are respectively arranged at the bottoms of the primary chromatographic column and the secondary chromatographic column, liquid leading pipes and liquid discharging pipes are respectively and fixedly connected to the outer parts of the three-way valves, and a charging tank is arranged at the top of the chromatographic assembly. According to the invention, the secondary chromatographic column is arranged, the liquid guide pipe of the primary chromatographic column is introduced into the secondary chromatographic column for secondary chromatography, and the solution after the secondary chromatography is introduced into the evaporation tank for evaporation and concentration and then introduced into the secondary chromatographic column for circulating chromatography, so that the chromatographic separation effect is improved, and the extraction efficiency of cannabidiol is improved.)

1. A double-stage chromatographic column separation system for purifying cannabidiol in industrial cannabis sativa comprises a chromatographic assembly (1) and is characterized in that: the chromatography component (1) comprises a primary chromatography column (11) and a secondary chromatography column (12), the primary chromatography column (11) and the secondary chromatography column (12) are fixedly connected through a fixing frame (2), liquid adding ports (13) are arranged at the tops of the primary chromatography column (11) and the secondary chromatography column (12), three-way valves (14) are arranged at the bottoms of the primary chromatography column (11) and the secondary chromatography column (12), liquid guide pipes (15) and liquid discharge pipes (16) are fixedly connected to the outer portions of the three-way valves (14), a feeding tank (3) is arranged at the top of the chromatography component (1), the bottom of the feeding tank (3) is connected to the liquid adding ports (13) at the top of the primary chromatography column (11) through pipelines, the liquid guide pipes (15) at the bottom of the primary chromatography column (11) are communicated to the liquid adding ports (13) at the top of the secondary chromatography column (12), and the liquid guide pipes (15) at the bottom of the secondary chromatography column (12) are connected with an evaporation tank (4), a liquid outlet at the bottom of the evaporation tank (4) is connected with a drainage pump (5) through a pipeline, and a liquid outlet of the drainage pump (5) is communicated with a liquid adding port (13) at the top of the secondary chromatographic column (12) through a pipeline.

2. The dual stage chromatography column separation system for cannabidiol purification from industrial cannabis as claimed in claim 1, wherein: and a first control valve (31) is arranged in a connecting pipeline between the bottom of the feeding tank (3) and the primary chromatographic column (11).

3. The dual stage chromatography column separation system for cannabidiol purification from industrial cannabis as claimed in claim 1, wherein: and a booster pump (6) is fixedly connected in a connecting pipeline of the feeding tank (3) and the primary chromatographic column (11).

4. The dual stage chromatography column separation system for cannabidiol purification from industrial cannabis as claimed in claim 1, wherein: and a second control valve (41) is fixedly connected in a connecting pipeline of the evaporation tank (4) and the drainage pump (5).

5. The dual stage chromatography column separation system for cannabidiol purification from industrial cannabis as claimed in claim 1, wherein: collecting grooves (7) are formed in the bottoms of the primary chromatographic column (11) and the secondary chromatographic column (12), and the liquid discharge pipe (16) is aligned with openings of the collecting grooves (7).

6. The dual stage chromatography column separation system for cannabidiol purification from industrial cannabis as claimed in claim 1, wherein: the fixing frame (2) comprises two clamping frames (21), and clamping grooves (22) are formed in the inner sides of the two clamping frames (21).

7. The dual-stage chromatography column separation system for cannabidiol purification from industrial cannabis as claimed in claim 6, wherein: two the one of them one end of holding frame (21) is passed through the hinge and is rotated the connection, and other end fixedly connected with locking plate (23), another of one of them holding frame (21) the other end of holding frame (21) is rotated and is installed threaded rod (25), locked groove (24) have been seted up to the inside of locking plate (23), threaded rod (25) block in the inside of locked groove (24), just the external thread of threaded rod (25) has cup jointed screw lock sleeve (26), the outer wall diameter value of screw lock sleeve (26) is greater than the width value of locked groove (24).

Technical Field

The invention relates to the technical field of chromatographic separation, in particular to a double-stage chromatographic column separation system for purifying cannabidiol in industrial hemp.

Background

The invention discloses a Chinese patent with publication number CN110317126A, which discloses a method for extracting cannabidiol by a microwave-assisted subcritical water extraction technology, belonging to the field of industrial cannabis, and comprising the following steps: the method comprises the following steps: freezing fresh industrial hemp plants and directly crushing the frozen fresh industrial hemp plants; step two: introducing water into crushed industrial hemp plants for microwave-assisted subcritical water extraction, wherein during microwave extraction, the microwave frequency is controlled to be 300-3000MHz, the power is controlled to be 200-1200W, the water temperature is controlled to be 100-374 ℃, the extraction pressure is 10-22 MPa, extraction is carried out for 10-60 minutes each time, water is recovered by evaporation from the obtained liquid phase after extraction is finished each time, and the cannabidiol concentrated solution is obtained after extraction is carried out for three times; step three: diluting the cannabidiol concentrated solution, performing gradient elution on the diluted cannabidiol concentrated solution through a chromatographic column, and collecting target eluent; concentrating and crystallizing the target eluent to obtain a cannabidiol product; the invention also discloses a system for carrying out the extraction process, wherein the prepared concentrated CBD solution is diluted by adding pure water, column chromatography gradient elution is needed, target eluent is collected, concentrated and crystallized to obtain a CBD product;

the prior art has the following defects: in the existing chromatographic separation system, separate chromatographic columns are mostly adopted for separation, the separation effect is poor, and the separation efficiency is low.

Disclosure of Invention

The invention aims to provide a double-stage chromatographic column separation system for purifying cannabidiol in industrial hemp, which aims to solve the defects in the prior art.

In order to achieve the above purpose, the invention provides the following technical scheme: a double-stage chromatographic column separation system for purifying cannabidiol in industrial cannabis comprises a chromatographic assembly, wherein the chromatographic assembly comprises a primary chromatographic column and a secondary chromatographic column, the primary chromatographic column and the secondary chromatographic column are fixedly connected through a fixing frame, liquid adding ports are formed in the tops of the primary chromatographic column and the secondary chromatographic column, three-way valves are arranged at the bottoms of the primary chromatographic column and the secondary chromatographic column, liquid guiding pipes and liquid discharging pipes are fixedly connected to the outer portions of the three-way valves, a feeding tank is arranged at the top of the chromatographic assembly, the bottom of the feeding tank is connected to the liquid adding port in the top of the primary chromatographic column through a pipeline, the liquid guiding pipe at the bottom of the primary chromatographic column is communicated to the liquid adding port in the top of the secondary chromatographic column, the liquid guiding pipe at the bottom of the secondary chromatographic column is connected with an evaporating tank, and a liquid outlet at the bottom of the evaporating tank is connected with a drainage pump through a pipeline, and a liquid outlet of the drainage pump is communicated with a liquid adding port at the top of the secondary chromatographic column through a pipeline.

Preferably, a first control valve is arranged in a connecting pipeline between the bottom of the feeding tank and the primary chromatographic column.

Preferably, a booster pump is fixedly connected in a connecting pipeline of the feeding tank and the primary chromatographic column.

Preferably, a second control valve is fixedly connected in a connecting pipeline of the evaporation tank and the drainage pump.

Preferably, collecting grooves are formed in the bottoms of the primary chromatographic column and the secondary chromatographic column, and the liquid discharge pipe is aligned with openings of the collecting grooves.

Preferably, the fixing frame comprises two clamping frames, and the inner sides of the two clamping frames are provided with clamping grooves.

Preferably, two wherein one end of holding frame is passed through the hinge and is rotated the connection, and the other end fixedly connected with locking plate of one of them holding frame, another the other end of holding frame is rotated and is installed the threaded rod, the locked groove has been seted up to the inside of locking plate, the threaded rod block is in the inside of locked groove, just the outside screw thread of threaded rod has cup jointed the screw lock cover, the outer wall diameter value of screw lock cover is greater than the width value of locked groove.

In the technical scheme, the invention provides the following technical effects and advantages:

1. when the device is actually used, the CBD solution is diluted in the feeding tank and then guided into the primary chromatographic column for primary chromatography, the secondary chromatographic column is arranged, the liquid guiding pipe of the primary chromatographic column is guided into the secondary chromatographic column, the solution part after primary chromatography of the primary chromatographic column can be further guided into the secondary chromatographic column for secondary chromatography, the evaporating tank is connected outside the liquid guiding pipe of the secondary chromatographic column, the solution after secondary chromatography is guided into the evaporating tank, and after evaporation and concentration are carried out by the evaporating tank, the solution part is further guided into the secondary chromatographic column for circulating chromatography by the flow guiding pump, so that repeated chromatographic separation is carried out on the solution part, the chromatographic separation effect is greatly improved, and the extraction efficiency of cannabidiol is further improved;

2. according to the invention, the first-stage chromatographic column and the second-stage chromatographic column can be respectively clamped between the two groups of clamping grooves by utilizing the hinging of the two clamping frames, and the locking plate and the threaded rod are arranged at the outer ends of the two clamping frames, after the two clamping frames are closed, the threaded rod is rotated into the locking groove to be clamped, and the threaded locking sleeve is pressed towards the locking plate by rotating the threaded locking sleeve, so that the two clamping frames are locked, after the separation is finished, the threaded locking sleeve can be rotated reversely, the threaded rod is turned out quickly, the clamping frames can be separated quickly, and the first-stage chromatographic column and the second-stage chromatographic column are separated, so that the internal substances are extracted, and the convenience and the practicability of the system use are further improved.

Drawings

In order to more clearly illustrate the embodiments of the present application or technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments described in the present invention, and other drawings can be obtained by those skilled in the art according to the drawings.

Fig. 1 is an overall configuration diagram of the system of the present invention.

Fig. 2 is a top view of the fixing frame of the present invention.

Description of reference numerals:

1. a chromatographic assembly; 11. a first-order chromatographic column; 12. a second-stage chromatographic column; 13. a liquid filling port; 14. a three-way valve; 15. a liquid guiding pipe; 16. a liquid discharge pipe; 2. a fixed mount; 21. a clamping frame; 22. a clamping groove; 23. a locking plate; 24. locking the groove; 25. a threaded rod; 26. a threaded lock sleeve; 3. a charging tank; 31. a first control valve; 4. An evaporator tank; 41. a second control valve; 5. a drainage pump; 6. a booster pump; 7. and (4) collecting the tank.

Detailed Description

In order to make the technical solutions of the present invention better understood, those skilled in the art will now describe the present invention in further detail with reference to the accompanying drawings.

The invention provides a double-stage chromatographic column separation system for purifying cannabidiol in industrial hemp, which comprises a chromatographic assembly 1, wherein the chromatographic assembly 1 comprises a primary chromatographic column 11 and a secondary chromatographic column 12, the primary chromatographic column 11 and the secondary chromatographic column 12 are fixedly connected through a fixing frame 2, liquid adding ports 13 are respectively arranged at the tops of the primary chromatographic column 11 and the secondary chromatographic column 12, three-way valves 14 are respectively arranged at the bottoms of the primary chromatographic column 11 and the secondary chromatographic column 12, liquid guide pipes 15 and liquid discharge pipes 16 are respectively and fixedly connected with the outer parts of the three-way valves 14, a feeding tank 3 is arranged at the top of the chromatographic assembly 1, the bottom of the feeding tank 3 is connected to the liquid adding port 13 at the top of the primary chromatographic column 11 through a pipeline, the liquid guide pipe 15 at the bottom of the primary chromatographic column 11 is communicated to the liquid adding port 13 at the top of the secondary chromatographic column 12, the liquid guide pipe 15 at the bottom of the secondary chromatographic column 12 is connected with an evaporating pot 4, a liquid outlet at the bottom of the evaporating pot 4 is connected with a drainage pump 5 through a pipeline, and a liquid outlet of the drainage pump 5 is communicated with a liquid adding port 13 at the top of the secondary chromatographic column 12 through a pipeline.

Further, in the above technical solution, a first control valve 31 is disposed in a connecting pipeline between the bottom of the feeding tank 3 and the primary chromatographic column 11, so as to regulate and control the flow rate of the solution filled in the primary chromatographic column 11.

Further, in the above technical scheme, a booster pump 6 is fixedly connected in the connecting pipeline of the feeding tank 3 and the primary chromatographic column 11, so that the chromatographic solution can be pressurized, and the chromatographic effect is improved.

Further, in the above technical solution, a second control valve 41 is fixedly connected to a connecting pipeline between the evaporation tank 4 and the drainage pump 5, so that the circulation flow rate can be controlled.

Further, in the above technical solution, the collecting groove 7 is provided at the bottom of the first-stage chromatographic column 11 and the second-stage chromatographic column 12, and the drain pipe 16 is aligned with the opening of the collecting groove 7, so as to facilitate the collection of the solution.

Further, in the above technical solution, the fixing frame 2 includes two holding frames 21, and the inner sides of the two holding frames 21 are both provided with holding grooves 22.

Further, in the above technical solution, one end of each of the two clamping frames 21 is rotatably connected through a hinge, the other end of one of the clamping frames 21 is fixedly connected with a locking plate 23, the other end of the other of the clamping frames 21 is rotatably provided with a threaded rod 25, a locking groove 24 is formed in the locking plate 23, the threaded rod 25 is clamped in the locking groove 24, a threaded locking sleeve 26 is sleeved on an external thread of the threaded rod 25, and the diameter value of the outer wall of the threaded locking sleeve 26 is greater than the width value of the locking groove 24;

the implementation mode is specifically as follows: in practical use, the CBD solution is diluted in the feeding tank 3, and then guided to the first-stage chromatographic column 11 for first-stage chromatography, and the solution after the first-stage chromatographic column 11 is primarily chromatographed by arranging the second-stage chromatographic column 12, and the liquid guiding tube 15 of the first-stage chromatographic column 11 is guided to the second-stage chromatographic column 12, so that the solution after the first-stage chromatographic column 11 is primarily chromatographed can be partially guided to the second-stage chromatographic column 12 for second-stage chromatography, and the evaporation tank 4 is externally connected to the liquid guiding tube 15 of the second-stage chromatographic column 12, so that the solution after the second-stage chromatography is guided to the evaporation tank 4, and after the evaporation tank 4 is used for evaporation concentration, the solution is guided to the second-stage chromatographic column 12 again by the liquid guiding pump 5 for circulating chromatography, so that the solution is repeatedly chromatographically separated, thereby greatly improving the chromatographic separation effect, further improving the extraction efficiency of cannabidiol, and after the separation, the circulation is closed, and the three-way valve 14 is adjusted to discharge the solution in the first-stage chromatographic column 11 and the second-stage chromatographic column 12 into the collecting tank 7 and collect the solution The separation can be completed, and the first-stage chromatographic column 11 and the second-stage chromatographic column 12 are integrally supported by the arrangement of the fixing frame 2, and by the hinging of the two clamping frames 21, the primary and secondary chromatography columns 11 and 12 may be sandwiched between two sets of holding grooves 22, and by arranging the locking pieces 23 and the threaded rods 25 at the outer ends of the two clamping frames 21, after the two clamping frames 21 are closed, the threaded rod 25 is rotated to the locking groove 24 to be clamped, and the screw lock sleeve 26 is pressed towards the locking piece 23 by rotating the screw lock sleeve 26, thereby locking the two clamping frames 21, and after the separation is finished, the threaded locking sleeve 26 can be rotated reversely to quickly turn out the threaded rod 25, the holding frame 21 can be quickly separated, the first-stage chromatographic column 11 and the second-stage chromatographic column 12 are separated, thereby extracting the internal substances and further improving the convenience and the practicability of the system.

While certain exemplary embodiments of the present invention have been described above by way of illustration only, it will be apparent to those of ordinary skill in the art that the described embodiments may be modified in various different ways without departing from the spirit and scope of the invention. Accordingly, the drawings and description are illustrative in nature and should not be construed as limiting the scope of the invention.