CN113577824B - Two-stage chromatographic column separation system for purifying cannabidiol in industrial cannabis - Google Patents
Two-stage chromatographic column separation system for purifying cannabidiol in industrial cannabis Download PDFInfo
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- CN113577824B CN113577824B CN202111028301.1A CN202111028301A CN113577824B CN 113577824 B CN113577824 B CN 113577824B CN 202111028301 A CN202111028301 A CN 202111028301A CN 113577824 B CN113577824 B CN 113577824B
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- QHMBSVQNZZTUGM-UHFFFAOYSA-N Trans-Cannabidiol Natural products OC1=CC(CCCCC)=CC(O)=C1C1C(C(C)=C)CCC(C)=C1 QHMBSVQNZZTUGM-UHFFFAOYSA-N 0.000 title claims abstract description 26
- QHMBSVQNZZTUGM-ZWKOTPCHSA-N cannabidiol Chemical compound OC1=CC(CCCCC)=CC(O)=C1[C@H]1[C@H](C(C)=C)CCC(C)=C1 QHMBSVQNZZTUGM-ZWKOTPCHSA-N 0.000 title claims abstract description 26
- 229950011318 cannabidiol Drugs 0.000 title claims abstract description 26
- ZTGXAWYVTLUPDT-UHFFFAOYSA-N cannabidiol Natural products OC1=CC(CCCCC)=CC(O)=C1C1C(C(C)=C)CC=C(C)C1 ZTGXAWYVTLUPDT-UHFFFAOYSA-N 0.000 title claims abstract description 26
- PCXRACLQFPRCBB-ZWKOTPCHSA-N dihydrocannabidiol Natural products OC1=CC(CCCCC)=CC(O)=C1[C@H]1[C@H](C(C)C)CCC(C)=C1 PCXRACLQFPRCBB-ZWKOTPCHSA-N 0.000 title claims abstract description 22
- 238000000926 separation method Methods 0.000 title claims abstract description 21
- 240000004308 marijuana Species 0.000 title abstract 2
- 239000007788 liquid Substances 0.000 claims abstract description 43
- 238000001704 evaporation Methods 0.000 claims abstract description 20
- 230000008020 evaporation Effects 0.000 claims abstract description 20
- 241000218236 Cannabis Species 0.000 claims description 13
- 238000004587 chromatography analysis Methods 0.000 abstract description 16
- 238000013375 chromatographic separation Methods 0.000 abstract description 8
- 238000000605 extraction Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000012141 concentrate Substances 0.000 description 3
- 239000003480 eluent Substances 0.000 description 3
- 244000198134 Agave sisalana Species 0.000 description 2
- 235000011624 Agave sisalana Nutrition 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003809 water extraction Methods 0.000 description 2
- 238000004440 column chromatography Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
Classifications
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/82—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by solid-liquid treatment; by chemisorption
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/16—Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention discloses a two-stage chromatographic column separation system for purifying cannabidiol in industrial cannabis, which relates to the technical field of chromatographic separation and comprises a chromatographic component, wherein the chromatographic component comprises a first-stage chromatographic column and a second-stage chromatographic column, the first-stage chromatographic column and the second-stage chromatographic column are fixedly connected through a fixing frame, liquid filling ports are formed in the tops of the first-stage chromatographic column and the second-stage chromatographic column, three-way valves are arranged at the bottoms of the first-stage chromatographic column and the second-stage chromatographic column, a liquid guiding pipe and a liquid draining pipe are fixedly connected to the outer parts of the three-way valves, and a material adding tank is arranged at the top of the chromatographic component. According to the invention, the secondary chromatographic column is arranged, the liquid guiding pipe of the primary chromatographic column is led into the secondary chromatographic column for secondary chromatography, and the solution after the secondary chromatography is led into the evaporation tank for evaporation concentration and then led into the secondary chromatographic column for circulating chromatography, so that the chromatographic separation effect is improved, and the extraction efficiency of cannabidiol is improved.
Description
Technical Field
The invention relates to the technical field of chromatographic separation, in particular to a two-stage chromatographic column separation system for purifying cannabidiol in industrial cannabis.
Background
One Chinese patent of the invention with publication number CN110317126A discloses a method for extracting cannabidiol by using a microwave-assisted subcritical water extraction technology, which belongs to the field of industrial cannabis and comprises the following steps: step one: freezing fresh industrial hemp plants and directly crushing; step two: introducing water into crushed industrial hemp plants for microwave-assisted subcritical water extraction, wherein during the 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, each time of extraction is 10-60 minutes, after each time of extraction is finished, water is evaporated and recovered from the obtained liquid phase, and after three times of repeated extraction, cannabidiol concentrate is obtained; step three: diluting the cannabidiol concentrate, performing gradient elution on the diluted cannabidiol concentrate through a chromatographic column, and collecting a 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 and then subjected to column chromatography gradient elution, and the 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, a single chromatographic column is adopted for separation, the separation effect is poor, and the separation efficiency is low.
Disclosure of Invention
The invention aims to provide a two-stage chromatographic column separation system for purifying cannabidiol in industrial cannabis, which solves the defects in the prior art.
In order to achieve the above object, the present invention provides the following technical solutions: the utility model provides a purifying cannabidiol's doublestage chromatographic column separation system in industry cannabis, includes the chromatography subassembly, the chromatography subassembly includes one-level chromatographic column and second grade chromatographic column, one-level chromatographic column and second grade chromatographic column pass through mount fixed connection, the top of one-level chromatographic column and second grade chromatographic column all is provided with the liquid filling port, the bottom of one-level chromatographic column and second grade chromatographic column all is provided with the three-way valve, the equal fixedly connected with liquid guiding pipe of outside of three-way valve and fluid-discharge tube, the top of chromatography subassembly is provided with the charging tank, the liquid filling port at one-level chromatographic column top is passed through the pipe connection to the bottom of charging tank, the liquid guiding pipe at one-level chromatographic column bottom communicates to the liquid filling port at second grade chromatographic column top, the liquid guiding pipe at second grade chromatographic column bottom is connected with the evaporation jar, the bottom liquid outlet of evaporation jar has the drainage pump through the pipe connection, the liquid outlet of drainage pump passes through the liquid pipe and the liquid filling port intercommunication at second grade chromatographic column top.
Preferably, a first control valve is arranged in a connecting pipeline between the bottom of the charging tank and the first-stage chromatographic column.
Preferably, a booster pump is fixedly connected in a connecting pipeline of the charging tank and the first-stage chromatographic column.
Preferably, a second control valve is fixedly connected in a connecting pipeline of the evaporation tank and the drainage pump.
Preferably, the bottoms of the primary chromatographic column and the secondary chromatographic column are provided with collecting tanks, and the liquid discharge pipe is aligned with the openings of the collecting tanks.
Preferably, the fixing frame comprises two clamping frames, and clamping grooves are formed in the inner sides of the two clamping frames.
Preferably, one end of each clamping frame is rotationally connected through a hinge, the other end of one clamping frame is fixedly connected with a locking plate, the other end of the clamping frame is rotationally provided with a threaded rod, a locking groove is formed in the locking plate, the threaded rod is clamped in the locking groove, a threaded lock sleeve is sleeved on an external thread of the threaded rod, and the diameter value of the outer wall of the threaded lock sleeve is larger than the width value of the locking groove.
In the technical scheme, the invention has the technical effects and advantages that:
1. In actual use, the CBD solution is diluted in the charging tank and then is guided into the first-stage chromatographic column for first-stage chromatography, the liquid guiding pipe of the first-stage chromatographic column is arranged and guided into the second-stage chromatographic column, so that the solution part after primary chromatography of the first-stage chromatographic column is guided into the second-stage chromatographic column for second-stage chromatography, the evaporation tank is connected outside the liquid guiding pipe of the second-stage chromatographic column, the solution after the second-stage chromatography is guided into the evaporation tank, the evaporation tank is utilized for evaporation concentration, and then the solution part is guided into the second-stage chromatographic column for circulating chromatography through the drainage pump, thereby repeatedly performing chromatographic separation on the solution part, further greatly improving the chromatographic separation effect and further improving the extraction efficiency of cannabidiol;
2. According to the invention, the primary chromatographic column and the secondary chromatographic column can be respectively clamped between the two groups of clamping grooves by utilizing the hinging of the two clamping frames, the locking plate and the threaded rod are arranged at the outer ends of the two clamping frames, the threaded rod is rotated into the locking groove to be clamped after the two clamping frames are closed, the threaded lock sleeve is tightly pressed towards the locking plate by rotating the threaded lock sleeve, so that the two clamping frames are locked, the threaded lock sleeve can be reversely rotated after the separation is finished, the threaded rod can be quickly turned out, the clamping frames can be quickly separated, the primary chromatographic column and the secondary chromatographic column are separated, and therefore, the internal substances are extracted, and the convenience and the practicability of the system are further improved.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings required for the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only some embodiments described in the present application, and other drawings may be obtained according to these drawings for those skilled in the art.
Fig. 1 is a system overall structure diagram of the present invention.
Fig. 2 is a top view of the holder of the present invention.
Reference numerals illustrate:
1. A chromatographic component; 11. a first-stage chromatographic column; 12. a secondary chromatographic column; 13. a liquid adding port; 14. a three-way valve; 15. a liquid guiding pipe; 16. a liquid discharge pipe; 2. a fixing frame; 21. a clamping frame; 22. a clamping groove; 23. a locking plate; 24. a locking groove; 25. a threaded rod; 26. a threaded lock sleeve; 3. a charging tank; 31. a first control valve; 4. An evaporation tank; 41. a second control valve; 5. a drainage pump; 6. a booster pump; 7. a collection tank.
Detailed Description
In order to make the technical scheme of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the accompanying drawings.
The invention provides a two-stage chromatographic column separation system for purifying cannabidiol in industrial cannabis, which is shown in figures 1-2, and comprises a chromatographic component 1, wherein the chromatographic component 1 comprises a first-stage chromatographic column 11 and a second-stage chromatographic column 12, the first-stage chromatographic column 11 and the second-stage chromatographic column 12 are fixedly connected through a fixing frame 2, liquid inlets 13 are respectively arranged at the tops of the first-stage chromatographic column 11 and the second-stage chromatographic column 12, three-way valves 14 are respectively arranged at the bottoms of the first-stage chromatographic column 11 and the second-stage chromatographic column 12, liquid guiding pipes 15 and liquid draining pipes 16 are respectively fixedly connected to the outsides of the three-way valves 14, the top of the chromatographic component 1 is provided with a charging tank 3, the bottom of the charging tank 3 is connected to the liquid inlets 13 at the top of the first-stage chromatographic column 11 through a pipeline, the liquid guiding pipes 15 at the bottom of the first-stage chromatographic column 11 are communicated to the liquid inlets 13 at the top of the second-stage chromatographic column 12, the liquid guiding pipes 15 at the bottom of the second-stage chromatographic column 12 are respectively connected with evaporation tanks 4, liquid outlets at the bottoms of the evaporation tanks 4 are respectively connected with pumps 5 through pipelines, and the liquid draining pipes 5 are respectively communicated with the liquid outlets 13 at the tops of the second-stage chromatographic columns 12 through the liquid guiding pipelines.
Furthermore, in the above technical solution, the first control valve 31 is disposed in the connecting pipeline between the bottom of the charging 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.
Furthermore, in the above technical scheme, the booster pump 6 is fixedly connected in the connecting pipeline between the charging 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, the second control valve 41 is fixedly connected to the connecting pipeline between the evaporation tank 4 and the drainage pump 5, so as to control the circulation flow rate.
Further, in the above technical solution, the bottoms of the primary chromatographic column 11 and the secondary chromatographic column 12 are provided with the collecting tank 7, and the liquid discharge pipe 16 is aligned with the opening of the collecting tank 7, so as to facilitate the collection of the solution.
Further, in the above technical solution, the fixing frame 2 includes two clamping frames 21, and the inner sides of the two clamping frames 21 are provided with clamping grooves 22.
Further, in the above technical solution, one end of the two clamping frames 21 is rotatably connected through a hinge, the other end of one clamping frame 21 is fixedly connected with a locking plate 23, the other end of the other clamping frame 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, an external thread of the threaded rod 25 is sleeved with a threaded lock sleeve 26, and the diameter value of the outer wall of the threaded lock sleeve 26 is larger than the width value of the locking groove 24;
The implementation mode specifically comprises the following steps: in practical use, the CBD solution is diluted in the charging tank 3 and then is guided into the first-stage chromatographic column 11 for first-stage chromatography, the second-stage chromatographic column 12 is arranged, the liquid guiding pipe 15 of the first-stage chromatographic column 11 is guided into the second-stage chromatographic column 12, the solution part after the primary chromatography of the first-stage chromatographic column 11 is further guided into the second-stage chromatographic column 12 for second-stage chromatography, the evaporation tank 4 is connected outside the liquid guiding pipe 15 of the second-stage chromatographic column 12, the solution after the second-stage chromatography is guided into the evaporation tank 4, the evaporation tank 4 is utilized for evaporation concentration, and then is guided into the second-stage chromatographic column 12 for circulating chromatography through the drainage pump 5, so that the repeated chromatographic separation is carried out on the solution part, the chromatographic separation effect is greatly improved, the extraction efficiency of cannabidiol is further improved, and after the separation is finished, the circulation is closed, the solution in the first-stage chromatographic column 11 and the second-stage chromatographic column 12 is discharged into the collecting tank 7 and collected by adjusting the three-way valve 14, the separation work can be completed, the first-stage chromatographic column 11 and the second-stage chromatographic column 12 are integrally supported by arranging the fixing frame 2, the first-stage chromatographic column 11 and the second-stage chromatographic column 12 can be respectively clamped between two groups of clamping grooves 22 by hinging the two clamping frames 21, the locking plates 23 and the threaded rods 25 are arranged at the outer ends of the two clamping frames 21, the threaded rods 25 are rotated into the locking grooves 24 to be clamped after the two clamping frames 21 are closed, the threaded locking sleeve 26 is rotated to be tightly pressed against the locking plates 23 by rotating the threaded locking sleeve 26, the threaded rods 25 can be reversely rotated to be quickly flipped out after the separation is completed, the clamping frames 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 practicality 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 modifications may be made to the described embodiments in various different ways without departing from the spirit and scope of the invention. Accordingly, the drawings and description are to be regarded as illustrative in nature and not as restrictive of the scope of the invention, which is defined by the appended claims.
Claims (7)
1. A two-stage chromatographic column separation system for purifying cannabidiol in industrial cannabis, comprising a chromatographic component (1), characterized in that: the utility model provides a chromatographic component (1) is including one-level chromatographic column (11) and second grade chromatographic column (12), one-level chromatographic column (11) and second grade chromatographic column (12) pass through mount (2) fixed connection, the top of one-level chromatographic column (11) and second grade chromatographic column (12) all is provided with liquid filling port (13), the bottom of one-level chromatographic column (11) and second grade chromatographic column (12) all is provided with three-way valve (14), the equal fixedly connected with liquid drainage pipe (15) and fluid-discharge tube (16) of outside of three-way valve (14), the top of chromatographic component (1) is provided with charging tank (3), liquid filling port (13) at charging tank (3) bottom through pipe connection to one-level chromatographic column (11) top, liquid drainage pipe (15) at one-level chromatographic column (11) bottom communicate liquid filling port (13) to second grade chromatographic column (12) top, liquid drainage pipe (15) at second grade chromatographic column (12) bottom are connected with evaporation tank (4), the bottom of evaporation tank (4) is through connecting liquid filling port (5) with drain pump (5) through drain pump (13) at second grade of liquid filling port.
2. A two-stage chromatographic column separation system for purifying cannabidiol in industrial cannabis as claimed in claim 1, wherein: a first control valve (31) is arranged in a connecting pipeline between the bottom of the charging tank (3) and the primary chromatographic column (11).
3. A two-stage chromatographic column separation system for purifying cannabidiol in industrial cannabis as claimed in claim 1, wherein: a booster pump (6) is fixedly connected in a connecting pipeline between the feeding tank (3) and the primary chromatographic column (11).
4. A two-stage chromatographic column separation system for purifying cannabidiol in industrial cannabis as claimed in claim 1, wherein: a second control valve (41) is fixedly connected in a connecting pipeline of the evaporation tank (4) and the drainage pump (5).
5. A two-stage chromatographic column separation system for purifying cannabidiol in industrial cannabis as claimed in claim 1, wherein: the bottoms of the primary chromatographic column (11) and the secondary chromatographic column (12) are provided with a collecting tank (7), and the liquid discharge pipe (16) is aligned with the opening of the collecting tank (7).
6. A two-stage chromatographic column separation system for purifying cannabidiol in 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. A two-stage chromatographic column separation system for purifying cannabidiol in industrial cannabis as claimed in claim 6, wherein: two one end of each clamping frame (21) is rotationally connected through a hinge, the other end of one clamping frame (21) is fixedly connected with a locking plate (23), the other end of the clamping frame (21) is rotationally 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 lock sleeve (26) is sleeved on an external thread of the threaded rod (25), and the diameter value of the outer wall of the threaded lock sleeve (26) is larger than the width value of the locking groove (24).
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| CN202111028301.1A CN113577824B (en) | 2021-09-02 | 2021-09-02 | Two-stage chromatographic column separation system for purifying cannabidiol in industrial cannabis |
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| CN215781674U (en) * | 2021-09-02 | 2022-02-11 | 温州市金榜轻工机械有限公司 | Double-stage chromatographic column separation system for purifying cannabidiol in industrial cannabis sativa |
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| US20050011835A1 (en) * | 2003-07-17 | 2005-01-20 | Sigma-Aldrich Co. | High throughput flash purification stand and cartridge |
| CN101260336B (en) * | 2008-04-15 | 2011-09-14 | 中国矿业大学 | Dehydration and alcoholysis device for low deterioration coal |
| US9433909B2 (en) * | 2012-06-20 | 2016-09-06 | Uop Llc | Apparatus for retaining solid material in a radial flow reactor and method of making |
| CN106924995A (en) * | 2015-12-30 | 2017-07-07 | 中美华世通生物医药科技（武汉）有限公司 | Continuous chromatography system and chromatography method |
| CN205347275U (en) * | 2016-01-19 | 2016-06-29 | 神舟生物科技有限责任公司 | 10 refined extraction system of ubiquinone |
| CN207203536U (en) * | 2017-08-08 | 2018-04-10 | 固安鼎材科技有限公司 | A kind of column chromatography equipment |
| MX2020009335A (en) * | 2018-03-07 | 2020-12-03 | Socati Tech Oregon Llc | Continuous isolation of cannabidiol and conversion of cannabidiol to delta 8-tetrahydrocannabinol and delta 9-tetrahydrocannabinol . |
| CN109395427A (en) * | 2019-01-03 | 2019-03-01 | 湖州欧利生物科技有限公司 | A kind of environment-friendly type glabridin extraction element and its technique |
| CN109999924B (en) * | 2019-04-12 | 2023-10-13 | 长春工程学院 | A multi-link ion exchange experimental device |
| CN110270134A (en) * | 2019-05-31 | 2019-09-24 | 江苏哈工药机科技股份有限公司 | A kind of high-purity C BD isolates and purifies device and its isolation and purification method |
| CN210583782U (en) * | 2019-08-19 | 2020-05-22 | 青岛海洋生物医药研究院股份有限公司 | A Column Chromatography Integrated System for Continuous Sample Loading |
| CN110467521A (en) * | 2019-08-22 | 2019-11-19 | 哈尔滨工业大学 | A method for separating and purifying cannabidiol (CBD) from industrial hemp |
| CN211676417U (en) * | 2019-11-13 | 2020-10-16 | 上海华谊能源化工有限公司 | Chromatographic column and combined chromatographic column |
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