Continuous crystallization device for preparing cannabidiol crystals

Abstract

The utility model discloses a continuous crystallizing device for preparing cannabidiol crystals, which belongs to the technical field of pharmaceutical equipment and comprises a dissolving tank, a primary crystallizing tank, a primary dryer, a primary evaporator, a primary liquid collecting tank, a secondary crystallizing tank, a secondary dryer, a secondary evaporator, a secondary liquid collecting tank, an evaporative condenser, a solvent storage tank and a connecting pipeline. A crystal washing device, a concentric forward and reverse differential mechanism, a pressing stirring paddle, an upturning stirring paddle, a scraping plate, a filter screen gate valve and the like are arranged in each of the first-stage crystallizing tank and the second-stage crystallizing tank. According to the utility model, two times of crystallization can be realized, the phenomena that the formed crystals are easy to attach to the inner wall of the crystallization tank and the crystal grains are not uniform due to the decline of the quality of raw materials during the second time of crystallization can be effectively avoided, the crystallization yield of the crystals is improved, the full-closed continuous operation is realized, the management and control risk is reduced, the equipment investment is reduced, and the production cost is reduced.

Description

Technical Field

[0001] The utility model relates to the technical field of pharmaceutical equipment, in particular to a continuous crystallization device for preparing cannabidiol crystals. Background Art

[0002] Cannabidiol (CBD for short) is the main chemical component of the medicinal plant industrial hemp. It is extracted from female cannabis plants and is a non-addictive component in cannabis. It has pharmacological effects such as antispasmodic, anti-anxiety, and anti-inflammatory. At present, the preparation process of high-purity cannabidiol is mostly organic solvent extraction, molecular distillation or resin separation and purification, chromatographic separation to remove the harmful component tetrahydrocannabinol, and then cooling and crystallizing to obtain high-purity cannabidiol crystals. The existing industrial crystallization preparation process is carried out intermittently using multiple steps, and there is a problem of non-closed turnover of cannabidiol raw materials, which poses a regulatory risk. At the same time, cannabidiol crystallization is cooling crystallization, and mostly uses primary crystallization or repeated crystallization, and the crystal content yield is relatively low.

[0003] In view of this, it is necessary to develop a continuous crystallization device for preparing cannabidiol crystals to overcome the above problems. Utility Model Content

[0004] The technical problem to be solved by the utility model is to provide a continuous crystallization device for preparing cannabidiol crystals, which can enable cannabidiol crystals to be produced continuously and closed from raw materials to crystals, and the crystals are subjected to continuous two-stage crystallization, which can improve the yield of crystal content.

[0005] In order to solve the above technical problems, the technical solution adopted by the utility model is:

[0006] A continuous crystallization device for preparing cannabidiol crystals, comprising a dissolving tank, a primary crystallization tank, a primary dryer, a primary evaporator, a primary liquid collecting tank, a secondary crystallization tank, a secondary dryer, a secondary evaporator, a secondary liquid collecting tank, an evaporation condenser, a solvent storage tank and connecting pipelines;

[0007] The dissolving tank is connected to the primary crystallization tank; the primary crystallization tank is connected to the primary dryer; the bottom liquid outlet of the primary dryer is connected to the liquid inlet of the primary evaporator; the bottom concentrated liquid outlet of the primary evaporator is connected to the liquid inlet of the primary liquid collecting tank; the bottom liquid outlet of the primary liquid collecting tank is connected to the liquid inlet of the secondary crystallization tank; the secondary crystallization tank is connected to the secondary dryer; the bottom liquid outlet of the secondary dryer is connected to the liquid inlet of the secondary evaporator; the bottom concentrated liquid outlet of the secondary evaporator is connected to the secondary liquid collecting tank The first and second liquid collecting tanks are connected; the bottom outlet of the second liquid collecting tank is connected to the packaging equipment; the evaporative condenser is connected to the first evaporator and the second evaporator through a vacuum pipeline; the evaporative condenser is connected to the first crystallization tank and the second crystallization tank through a cold water pipeline; the first crystallization tank is connected to the cold water tank; the evaporative condenser is connected to the solvent storage tank; the solvent storage tank is connected to the first crystallization tank, the second crystallization tank and the dissolution tank; the first evaporator and the second evaporator are connected to the hot water pipeline; the second evaporator is connected to the hot water tank.

[0008] A further improvement of the technical solution of the utility model lies in that: a first pump is arranged on the connecting pipeline between the dissolving tank and the primary crystallization tank; a second pump is arranged between the bottom liquid outlet of the primary dryer and the liquid inlet of the primary evaporator; a third pump is arranged between the bottom liquid outlet of the primary liquid collecting tank and the liquid inlet of the secondary crystallization tank; a fourth pump is arranged between the bottom liquid outlet of the secondary dryer and the liquid inlet of the secondary evaporator; a fifth pump is arranged between the bottom outlet of the secondary liquid collecting tank and the packaging equipment; and a sixth pump is arranged on the connecting pipeline of the bottom liquid outlet of the dissolving tank.

[0009] A further improvement of the technical solution of the utility model is that the primary crystallization tank and the secondary crystallization tank have the same structure.

[0010] The further improvement of the technical solution of the utility model lies in that: the secondary crystallization tank comprises a tank body, a motor arranged on the top of the tank body, a shaft arranged inside the tank body and connected to the motor, a concentric forward and reverse differential arranged at the lower end of the motor, a liquid inlet arranged at the upper end of the tank body, a plurality of crystal washing spray ports arranged at the upper end of the tank body, a downward pressure stirring paddle arranged inside the tank body, an upward turning stirring paddle arranged inside the tank body, a scraper arranged on the inner wall of the tank body, and a filter gate valve arranged at the lower part of the bottom end of the tank body and capable of separating the filtrate and the crystals; a jacket for passing cold water is arranged outside the tank body, a jacket cold water outlet is arranged at the upper end of the jacket, and a jacket cold water inlet is arranged at the lower end of the jacket; the scraper is fixed to the shaft by a connecting rod, and the scraper, the downward pressure stirring paddle and the upward turning stirring paddle are controlled by the concentric forward and reverse differential to realize downward pressure, upward turning and forward and reverse rotation.

[0011] A further improvement of the technical solution of the utility model is that the secondary crystallization tank is also provided with a nitrogen inlet.

[0012] A further improvement of the technical solution of the utility model is that the primary dryer and the secondary dryer are both centrifugal dryers, and filter bags capable of taking out crystals are arranged inside.

[0013] A further improvement of the technical solution of the utility model is that: a jacket for passing hot water is arranged outside the tank body of the primary evaporator and the secondary evaporator.

[0014] Due to the adoption of the above technical solution, the technical progress achieved by the utility model is:

[0015] 1. The utility model adopts a primary crystallization tank and a secondary crystallization tank and a dissolving tank, a dryer, an evaporator, a liquid collecting tank, an evaporative condenser, a solvent storage tank and corresponding cold water pipelines, hot water pipelines, vacuum pipelines, etc. connected thereto, which can enable the cannabidiol raw material to achieve two-stage crystallization and improve the crystal content yield.

[0016] 2. The utility model adopts a primary crystallization tank and a secondary crystallization tank with the same structure, and a downward pressure stirring paddle, an upward turning stirring paddle and a scraper are arranged in the crystallization tank. The scraper, the downward pressure stirring paddle and the upward turning stirring paddle are reversely moved by a concentric forward and reverse differential, so that the material circulates up and down and left and right, which can prevent the crystals from adhering to the inner wall of the crystallization tank and preventing the crystals from scaling inside the crystallization tank, thereby ensuring that the grain size and shape are uniform.

[0017] 3. In the utility model, a crystal washing spray port and a filter gate valve are arranged in the crystallization tank, which can separate the crystal from the filtrate and realize secondary crystal washing. The crystal washing, crystallization and filtration processes can be completed in one device, which reduces equipment investment and shortens operation time.

[0018] 4. The utility model can realize fully enclosed production from raw materials to products by connecting various devices, reducing monitoring risks and avoiding leakage of organic solvents.

[0019] 5. The utility model has a simple structure, is safe and standardized, can reduce production costs and improve product yields. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] In order to more clearly illustrate the embodiments of the utility model or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art are briefly introduced below. Obviously, the drawings described below are some embodiments of the utility model. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative labor;

[0021] Figure 1It is a schematic diagram of the structure of a continuous crystallization device for preparing cannabidiol crystals provided in an embodiment of the utility model;

[0022] Figure 2 This is a schematic diagram of the structure of a crystallization tank in an embodiment of the utility model;

[0023] Among them, 1. dissolving tank; 2. primary crystallization tank; 3. primary dryer; 4. primary evaporator; 5. primary liquid collecting tank; 6. secondary crystallization tank; 6-1. motor; 6-2. concentric forward and reverse differential; 6-3. liquid inlet; 6-4. crystal washing spray port; 6-5. downward pressure stirring paddle; 6-6. upward turning stirring paddle; 6-7. scraper; 6-8. filter gate valve; 6-9. jacket cold water outlet; 6-10. jacket cold water inlet; 7. secondary dryer; 8. secondary evaporator; 9. secondary liquid collecting tank; 10. evaporative condenser; 11. solvent storage tank. DETAILED DESCRIPTION

[0024] It should be noted that the terms "including" and "having" and any variations thereof in the specification and claims of the present invention and the above-mentioned drawings are intended to cover non-exclusive inclusions. For example, a process, method, system, product or device that includes a series of steps or units is not necessarily limited to those steps or units clearly listed, but may include other steps or units that are not clearly listed or inherent to these processes, methods, products or devices.

[0025] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present invention.

[0026] In addition, the terms "first" and "second" are used for descriptive purposes only and cannot be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include at least one of the features. In the description of the present utility model, the meaning of "several" is at least two, such as two, three, etc., unless otherwise clearly and specifically defined.

[0027] The present invention is further described in detail below with reference to the accompanying drawings and embodiments:

[0028] like Figure 1As shown, a continuous crystallization device for preparing cannabidiol crystals includes a dissolving tank 1, a primary crystallization tank 2, a primary dryer 3, a primary evaporator 4, a primary liquid collecting tank 5, a secondary crystallization tank 6, a secondary dryer 7, a secondary evaporator 8, a secondary liquid collecting tank 9, an evaporation condenser 10, a solvent storage tank 11 and connecting pipelines;

[0029] The dissolving tank 1 is connected to the primary crystallizing tank 2; the primary crystallizing tank 2 is connected to the primary dryer 3; the bottom liquid outlet of the primary dryer 3 is connected to the liquid inlet of the primary evaporator 4; the bottom concentrated liquid outlet of the primary evaporator 4 is connected to the liquid inlet of the primary liquid collecting tank 5; the bottom liquid outlet of the primary liquid collecting tank 5 is connected to the liquid inlet of the secondary crystallizing tank 6; the secondary crystallizing tank 6 is connected to the secondary dryer 7; the bottom liquid outlet of the secondary dryer 7 is connected to the liquid inlet of the secondary evaporator 8; the bottom concentrated liquid outlet of the secondary evaporator 8 is connected to the secondary liquid collecting tank 9 The bottom outlet of the secondary liquid collecting tank 9 is connected to the packaging equipment; the evaporative condenser 10 is connected to the primary evaporator 4 and the secondary evaporator 8 through a vacuum pipeline; the evaporative condenser 10 is connected to the primary crystallization tank 2 and the secondary crystallization tank 6 through a cold water pipeline; the primary crystallization tank 2 is connected to the cold water tank; the evaporative condenser 10 is connected to the solvent storage tank 11; the solvent storage tank 11 is connected to the primary crystallization tank 2, the secondary crystallization tank 6 and the dissolution tank 1; the primary evaporator 4 and the secondary evaporator 8 are connected to the hot water pipeline; the secondary evaporator 8 is connected to the hot water tank.

[0030] Furthermore, a first pump is arranged on the connecting pipeline between the dissolving tank 1 and the primary crystallization tank 2; a second pump is arranged between the bottom liquid outlet of the primary dryer 3 and the liquid inlet of the primary evaporator 4; a third pump is arranged between the bottom liquid outlet of the primary liquid collecting tank 5 and the liquid inlet of the secondary crystallization tank 6; a fourth pump is arranged between the bottom liquid outlet of the secondary dryer 7 and the liquid inlet of the secondary evaporator 8; a fifth pump is arranged between the bottom outlet of the secondary liquid collecting tank 9 and the packaging equipment; and a sixth pump is arranged on the solvent pipeline of the bottom liquid outlet of the dissolving tank 1.

[0031] Further, the primary crystallization tank 2 and the secondary crystallization tank 6 have the same structure. A jacket connected to the cold water pipeline is provided outside the primary crystallization tank 2 and the secondary crystallization tank 6. The cold water flows into the jacket of the secondary crystallization tank 6 after passing through the evaporative condenser 10, and then flows into the jacket of the primary crystallization tank 2. The cold water flows out of the jacket of the primary crystallization tank 2 and returns to the cold water tank.

[0032] Further, such as Figure 2As shown, the secondary crystallization tank 6 includes a tank body, a motor 6-1 arranged on the top of the tank body, a shaft arranged inside the tank body and connected to the motor 6-1, a concentric forward and reverse differential 6-2 arranged at the lower end of the motor 6-1, a liquid inlet 6-3 arranged at the upper end of the tank body, a crystal washing spray port 6-4 arranged at the upper end of the tank body, a downward pressure stirring paddle 6-5 arranged inside the tank body, an upward stirring paddle 6-6 arranged inside the tank body, a scraper 6-7 arranged on the inner wall of the tank body, and a filter gate valve 6-8 arranged at the lower part of the bottom end of the tank body; a jacket is arranged outside the tank body, a jacket cold water outlet 6-9 is arranged at the upper end of the jacket, and a jacket cold water inlet 6-10 is arranged at the lower end of the jacket; the filter gate valve 6-8 can separate the filtrate and the crystals. The scraper 6-7 is fixed on the shaft through a connecting rod, and the upward stirring paddle 6-6 is arranged at a distance below the lower end of the downward pressing stirring paddle 6-5; the scraper 6-7, the downward pressing stirring paddle 6-5 and the upward stirring paddle 6-6 are controlled by the concentric forward and reverse differential 6-2 to realize downward pressing, upward turning and forward and reverse rotation.

[0033] During the secondary crystallization process, the scraper 6-7, the downward stirring paddle 6-5 and the upward stirring paddle 6-6 move in opposite directions, so that the material circulates up and down and left and right to avoid scaling of crystals inside the crystallization tank and make the grain size uniform. After the secondary crystallization is completed, the crystallization filtrate is concentrated.

[0034] Furthermore, the secondary crystallization tank 6 is also provided with a nitrogen inlet. After the crystallization is completed, the crystals and the filtrate are separated into solid and liquid by nitrogen pressure, and the crystallization filtrate is firstly pumped into the primary dryer 3 (connected to the primary crystallization tank 2) or the secondary dryer 7 (connected to the secondary crystallization tank 6) through the pipeline after the filtration is completed through the filter gate valve 6-8 arranged at the bottom.

[0035] Furthermore, the second-stage dryer 7 and the second-stage dryer 7 are both centrifugal dryers, and a filter bag capable of taking out crystals is arranged inside.

[0036] Furthermore, jackets for hot water are provided outside the tanks of the primary evaporator 4 and the secondary evaporator 8. The jackets of the primary evaporator 4 and the secondary evaporator 8 are both connected to the hot water pipeline, and the hot water flows into the jacket of the secondary evaporator 8 after passing through the jacket of the primary evaporator 4, and the hot water flows out of the jacket of the secondary evaporator 8 and returns to the hot water tank. At the same time, the primary evaporator 4 and the secondary evaporator 8 can be evacuated through the evaporative condenser 10.

[0037] The process of preparing cannabidiol crystals is as follows:

[0038] Cannabidiol oil is pumped into a dissolving tank 1 for dissolution. After being filtered by a filter installed at the bottom of the dissolving tank 1, the impurity-free dissolving liquid is pumped into a primary crystallization tank 2 through a first pump. After crystallization is completed, the crystals are washed through a first spray device at the top of the primary crystallization tank 2 (a first filter gate valve arranged at the bottom of the primary crystallization tank 2 first pumps the crystallization mother liquor after filtering the crystals into a primary dryer 3, and then the crystals are washed, and so on). The filtrate (crystallization mother liquor and washing liquid) is first pumped into the primary dryer 3, and finally the crystals are also pumped into the primary dryer 3. The crystals are centrifugally dried in the primary dryer 3, and the dried crystals are taken out through a filter bag for product (crystal) packaging; the filtrate (crystallization mother liquor and washing liquid) is pumped into a primary evaporator 4 through a second pump to recover the solvent, and the solvent gas after heating and vacuum evaporation flows into a solvent storage tank 11 after passing through an evaporation condenser 10; the filtrate (crystallization mother liquor and washing liquid) after the solvent is recovered is pumped into a primary liquid collecting tank 5, and after being concentrated to a metering volume, it is pumped into a secondary crystallization tank 6 through a third pump for secondary crystallization;

[0039] After the crystallization is completed in the secondary crystallization tank 6, the crystals are washed by the second spray device (the filter gate valve 6-8 set at the bottom of the secondary crystallization tank 6 first injects the crystal mother liquor after filtering the crystals into the secondary dryer 7, and then washes the crystals, and so on), the filtrate (crystallization mother liquor and washing liquid) is first injected into the secondary dryer 7, and finally the crystals are also injected into the secondary dryer 7, the crystals are centrifugally dried in the secondary dryer 7, and the dried crystals are taken out through the filter bag for product (crystal) packaging; the filtrate (crystallization mother liquor and washing liquid) is injected into the primary evaporator 8 through the fourth pump to recover the solvent, and the solvent gas after heating and vacuum evaporation flows into the solvent storage tank 11 after passing through the evaporation condenser 10; the filtrate (crystallization mother liquor and washing liquid) after the solvent is recovered is injected into the secondary liquid collecting tank 9, and the "full spectrum oil" collected in the secondary liquid collecting tank 9 is sent to the packaging equipment for packaging. The whole device can produce two products: crystals and full spectrum oil.

[0040] The solvent recovered by the solvent storage tank 11 can be returned to the dissolution tank 1, the primary crystallization tank 2 and the secondary crystallization tank 6 for reuse.

[0041] In summary, the continuous crystallization device provided by the utility model can realize two crystallizations, and can effectively avoid the second crystallization due to the decline in raw material quality, the formed crystals are easy to adhere to the inner wall of the crystallization tank, and the grains are uneven, thereby improving the crystallization yield, fully enclosed, continuous operation, reducing management and control risks, reducing equipment investment, and reducing production costs.

[0042] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the utility model, rather than to limit it. Although the utility model has been described in detail with reference to the aforementioned embodiments, ordinary technicians in this field should understand that they can still modify the technical solutions recorded in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not make the essence of the corresponding technical solution deviate from the scope of the technical solution of the embodiments of the utility model.

Claims

1. A continuous crystallization device for preparing cannabidiol crystals, characterized in that: It comprises a dissolving tank (1), a primary crystallizing tank (2), a primary dryer (3), a primary evaporator (4), a primary liquid collecting tank (5), a secondary crystallizing tank (6), a secondary dryer (7), a secondary evaporator (8), a secondary liquid collecting tank (9), an evaporation condenser (10), a solvent storage tank (11) and connecting pipelines; The dissolving tank (1) is connected to the primary crystallizing tank (2); the primary crystallizing tank (2) is connected to the primary dryer (3); the bottom liquid outlet of the primary dryer (3) is connected to the liquid inlet of the primary evaporator (4); the bottom concentrated liquid outlet of the primary evaporator (4) is connected to the liquid inlet of the primary liquid collecting tank (5); the bottom liquid outlet of the primary liquid collecting tank (5) is connected to the liquid inlet of the secondary crystallizing tank (6); the secondary crystallizing tank (6) is connected to the secondary dryer (7); the bottom liquid outlet of the secondary dryer (7) is connected to the liquid inlet of the secondary evaporator (8); the bottom concentrated liquid outlet of the secondary evaporator (8) is connected to the secondary liquid collecting tank (9); The bottom outlet of the secondary liquid collecting tank (9) is connected to the packaging equipment; the evaporative condenser (10) is connected to the primary evaporator (4) and the secondary evaporator (8) through a vacuum pipeline; the evaporative condenser (10) is connected to the primary crystallization tank (2) and the secondary crystallization tank (6) through a cold water pipeline; the primary crystallization tank (2) is connected to the cold water tank; the evaporative condenser (10) is connected to the solvent storage tank (11); the solvent storage tank (11) is connected to the primary crystallization tank (2), the secondary crystallization tank (6) and the dissolution tank (1); the primary evaporator (4) and the secondary evaporator (8) are connected to a hot water pipeline; the secondary evaporator (8) is connected to a hot water tank.

2. A continuous crystallization device for preparing cannabidiol crystals according to claim 1, characterized in that: A first pump is provided on the connecting pipeline between the dissolving tank (1) and the primary crystallizing tank (2); a second pump is provided between the bottom liquid outlet of the primary dryer (3) and the liquid inlet of the primary evaporator (4); a third pump is provided between the bottom liquid outlet of the primary collecting tank (5) and the liquid inlet of the secondary crystallizing tank (6); a fourth pump is provided between the bottom liquid outlet of the secondary dryer (7) and the liquid inlet of the secondary evaporator (8); a fifth pump is provided between the bottom outlet of the secondary collecting tank (9) and the packaging equipment; and a sixth pump is provided on the connecting pipeline of the bottom liquid outlet of the dissolving tank (1).

3. A continuous crystallization device for preparing cannabidiol crystals according to claim 1, characterized in that: The primary crystallization tank (2) and the secondary crystallization tank (6) have the same structure.

4. A continuous crystallization device for preparing cannabidiol crystals according to claim 3, characterized in that: The secondary crystallization tank (6) comprises a tank body, a motor (6-1) arranged on the top of the tank body, a shaft arranged inside the tank body and connected to the motor (6-1), a concentric forward and reverse differential (6-2) arranged at the lower end of the motor (6-1), a liquid inlet (6-3) arranged at the upper end of the tank body, a plurality of crystal washing spray ports (6-4) arranged at the upper end of the tank body, a downward pressure stirring paddle (6-5) arranged inside the tank body, an upward turning stirring paddle (6-6) arranged inside the tank body, and a scraper (6-7) arranged on the inner wall of the tank body. , a filter gate valve (6-8) is arranged at the lower part of the bottom end of the tank body and can separate the filtrate and the crystals; a jacket for passing cold water is arranged outside the tank body, a jacket cold water outlet (6-9) is arranged at the upper end of the jacket, and a jacket cold water inlet (6-10) is arranged at the lower end of the jacket; the scraper (6-7) is fixed to the shaft through a connecting rod, and the scraper (6-7), the downward pressure stirring paddle (6-5) and the upward turning stirring paddle (6-6) are controlled by a concentric forward and reverse differential (6-2) to realize downward pressure, upward turning and forward and reverse rotation.

5. A continuous crystallization device for preparing cannabidiol crystals according to claim 4, characterized in that: The secondary crystallization tank (6) is also provided with a nitrogen inlet.

6. A continuous crystallization device for preparing cannabidiol crystals according to claim 1, characterized in that: The primary dryer (3) and the secondary dryer (7) are both centrifugal dryers, and filter bags capable of removing crystals are arranged inside.

7. A continuous crystallization device for preparing cannabidiol crystals according to claim 1, characterized in that: The first-stage evaporator (4) and the second-stage evaporator (8) are both provided with jackets outside the tanks for passing hot water.

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