CN207384906U - A chromatography device for extracting cannabidiol from industrial hemp - Google Patents
A chromatography device for extracting cannabidiol from industrial hemp Download PDFInfo
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Abstract
Description
技术领域technical field
本实用新型属于分离提纯设备技术领域,具体涉及一种用于工业大麻中提取大麻二酚的层析装置。The utility model belongs to the technical field of separation and purification equipment, in particular to a chromatographic device for extracting cannabidiol from industrial hemp.
背景技术Background technique
大麻二酚(CBD)是一种从工业大麻中提取的无毒的、可以食用并具有药用价值的高附加值的酚类物质,是大麻中的非成瘾成分,能阻碍THC对人体神经系统影响,并具有抗痉挛、抗风湿性关节炎、抗焦虑等药理活性。层析技术是目前制药、化工等领域中分离效率最高的方法之一,也是天然产物分离及其他高纯度物质制备分离的重要手段之一。Cannabidiol (CBD) is a non-toxic, edible and high-value-added phenolic substance extracted from industrial hemp. Systemic effects, and has pharmacological activities such as anti-spasmodic, anti-rheumatoid arthritis, and anti-anxiety. Chromatography technology is currently one of the most efficient separation methods in the fields of pharmacy and chemical industry, and it is also one of the important means for the separation of natural products and the preparation and separation of other high-purity substances.
粗提取的大麻二酚浸膏包含有多种化学成分,其中有许多不明化学成分在内,因此,使用受到许多限制。采用层析色谱技术进行纯化是得到高纯度CBD的首选,但是现有的层析设备还存在诸多问题,例如现有的层析装置,一部分是采用人工进行加液,不仅增加成本,而且由于层析周期长,大多需要长时间接触洗脱液,损害身体健康,一部分采用预先配好的洗脱液进行加液,但是由于液体挥发等因素的存在,使得洗脱液比例难以保持恒定,而且预先配置大量的洗脱液,在层析过程中难以根据实际情况随时调整洗脱液的配比,一旦调整配比,大量预配好的洗脱液作废,需要重新进行回收才能再次利用,费时费力。同时,在层析过程中,很容易由于配液设备故障而导致干柱现象,直接造成层析失败。而且现有的流动相之间并没有设置混合装置,使得流动相之间混合不均匀,进行洗脱时,洗脱剂比例不一致,也容易造成层析的失败。The crudely extracted cannabidiol extract contains a variety of chemical components, many of which are unknown, so the use is subject to many restrictions. Purification by chromatographic technology is the first choice to obtain high-purity CBD, but there are still many problems in the existing chromatographic equipment. The analysis period is long, and most of them need to contact the eluent for a long time, which will damage the health of the body. Some of them use the pre-prepared eluent to add liquid, but due to the existence of factors such as liquid volatilization, it is difficult to keep the eluent ratio constant, and A large number of eluents are configured, and it is difficult to adjust the ratio of eluents at any time during the chromatography process according to the actual situation. Once the ratio is adjusted, a large amount of pre-prepared eluents will be discarded and need to be recycled before they can be reused, which is time-consuming and laborious. . At the same time, during the chromatographic process, it is easy to cause dry column phenomenon due to the failure of liquid preparation equipment, which directly leads to chromatographic failure. Moreover, there is no mixing device between the existing mobile phases, so that the mixing between the mobile phases is uneven, and when elution is performed, the eluent ratio is inconsistent, and it is easy to cause chromatography failure.
因此,有必要开发一种用于工业大麻中提取大麻二酚的层析装置。Therefore, it is necessary to develop a chromatography device for extracting cannabidiol from industrial hemp.
实用新型内容Utility model content
本实用新型的目的在于提供一种用于工业大麻中提取大麻二酚的层析装置。The purpose of the utility model is to provide a chromatography device for extracting cannabidiol from industrial hemp.
本实用新型的目的是这样实现的,所述的层析装置包括配液装置、层析柱和控制器,所述的配液装置包括流动相A储罐、流动相B储罐、混合罐、加液罐,所述的流动相A储罐、流动相B储罐均与混合罐连接,所述的流动相A储罐与混合罐之间设置有流量控制阀A,所述的流动相B储罐与混合罐之间设置有流量控制阀B,所述的混合罐中设置有搅拌装置,所述的加液罐设置在混合罐的下方,所述的加液罐中设置有液体浓度传感器,所述的控制器电连接液体浓度传感器、流量控制阀A和流量控制阀B;所述的加液罐与层析柱之间通过输送泵加液,所述的层析柱包括进液口、柱体和出液口,所述的进液口下方设置有液流分布器。The purpose of the utility model is achieved in that the chromatographic device includes a liquid distribution device, a chromatography column and a controller, and the liquid distribution device includes a mobile phase A storage tank, a mobile phase B storage tank, a mixing tank, Liquid addition tank, the mobile phase A storage tank and the mobile phase B storage tank are connected to the mixing tank, a flow control valve A is arranged between the mobile phase A storage tank and the mixing tank, and the mobile phase B A flow control valve B is arranged between the storage tank and the mixing tank, the mixing tank is provided with a stirring device, the liquid adding tank is arranged under the mixing tank, and a liquid concentration sensor is arranged in the liquid adding tank , the controller is electrically connected to the liquid concentration sensor, the flow control valve A and the flow control valve B; the liquid addition tank and the chromatographic column are filled by a delivery pump, and the chromatographic column includes a liquid inlet , a column and a liquid outlet, and a liquid flow distributor is arranged below the liquid inlet.
与现有技术相比,本实用新型具有以下技术效果:Compared with the prior art, the utility model has the following technical effects:
1、本实用新型通过搅拌装置将流动相在混合罐中进行充分混合,并实时控制使得加液罐中的洗脱液配比稳定,提高层析过程的稳定性;同时,本实用新型还能够根据层析进程随时调整洗脱液的配比,避免了现有技术中预先配液的种种弊端,分离效率高,省时省力。1. The utility model fully mixes the mobile phase in the mixing tank through the stirring device, and real-time control makes the ratio of the eluent in the liquid addition tank stable, improving the stability of the chromatography process; at the same time, the utility model can also The ratio of the eluent is adjusted at any time according to the chromatographic process, which avoids various disadvantages of pre-preparation in the prior art, and has high separation efficiency and saves time and effort.
2、本实用新型通过在层析柱的进液口下方设置液流分布器,使得洗脱液分布均匀,操作稳定,有效提高分离效率;通过报警装置的设置,避免过柱过程中由于配液设备故障导致的干柱现象,有效提高过柱的成功率,便于产物的分离。2. The utility model arranges a liquid flow distributor under the liquid inlet of the chromatographic column, so that the eluent is evenly distributed, the operation is stable, and the separation efficiency is effectively improved; The dry column phenomenon caused by equipment failure can effectively improve the success rate of passing through the column and facilitate the separation of products.
3、本实用新型采用多个接液罐循环进行接液,大大降低分离后的高纯度大麻二酚与杂质复混的可能性,有效提高分离效率,便于直接得到高纯度的产物,同时便于单一流动相进行冲柱时的回收,简化工艺,降低成本。3. The utility model adopts a plurality of liquid-receiving tanks to circulate the liquid, which greatly reduces the possibility of compounding the separated high-purity cannabidiol and impurities, effectively improves the separation efficiency, and facilitates the direct obtaining of high-purity products. At the same time, it is convenient for single The recovery of the mobile phase during column flushing simplifies the process and reduces the cost.
4、本实用新型通过混合罐的设置,使得流动相之间混合均匀,大大提高了层析的成功率。4. The utility model makes the mobile phases mix evenly through the setting of the mixing tank, which greatly improves the success rate of chromatography.
5、本实用新型的不锈钢柱体能够适应工业生产的需要,同时可视窗的存在便于实时观察层析柱柱体的情况,当柱体内填料出现气泡、断层等情况时能够及时发现和调整,便于层析过程的控制。5. The stainless steel cylinder of the utility model can meet the needs of industrial production. At the same time, the existence of the visible window is convenient for real-time observation of the column of the chromatography column. When bubbles and faults appear in the filler in the column, it can be found and adjusted in time, which is convenient Control of the chromatographic process.
6、本实用新型结构简单,得到的产品纯度高,质量好,而且在一定程度上实现自动化,也大大减少了人工成本,环保节能,便于扩大化使用。6. The utility model has a simple structure, and the obtained product has high purity and good quality, and realizes automation to a certain extent, greatly reduces labor costs, is environmentally friendly and energy-saving, and is convenient for expanded use.
附图说明Description of drawings
图1为本实用新型的结构示意图;Fig. 1 is the structural representation of the utility model;
图2为本实用新型的原理示意图;Fig. 2 is the schematic diagram of the principle of the utility model;
图中:1-流动相A储罐、2-流动相B储罐、3-混合罐、4-加液罐、5-层析柱、6-流量控制阀A、7-流量控制阀B、8-搅拌装置、9-液体浓度传感器、10-液流分布器、11-液位传感器。In the figure: 1-mobile phase A storage tank, 2-mobile phase B storage tank, 3-mixing tank, 4-liquid addition tank, 5-chromatographic column, 6-flow control valve A, 7-flow control valve B, 8-stirring device, 9-liquid concentration sensor, 10-liquid flow distributor, 11-liquid level sensor.
具体实施方式Detailed ways
下面结合附图对本实用新型作进一步的说明,但不以任何方式对本实用新型加以限制,基于本实用新型教导所作的任何变换或替换,均属于本实用新型的保护范围。The utility model will be further described below in conjunction with the accompanying drawings, but the utility model is not limited in any way. Any transformation or replacement based on the teaching of the utility model belongs to the protection scope of the utility model.
如附图1~图2所示的层析装置包括配液装置、层析柱5和控制器,所述的配液装置包括流动相A储罐1、流动相B储罐2、混合罐3、加液罐4,所述的流动相A储罐1、流动相B储罐2均与混合罐3连接,所述的流动相A储罐1与混合罐3之间设置有流量控制阀A6,所述的流动相B储罐2与混合罐3之间设置有流量控制阀B7,所述的混合罐3中设置有搅拌装置8,所述的加液罐4设置在混合罐3的下方,所述的加液罐4中设置有液体浓度传感器9,所述的控制器电连接液体浓度传感器9、流量控制阀A6和流量控制阀B7;所述的加液罐4与层析柱5之间通过输送泵加液,所述的层析柱5包括进液口、柱体和出液口,所述的进液口下方设置有液流分布器10。The chromatographic device as shown in accompanying drawings 1 to 2 includes a liquid distribution device, a chromatography column 5 and a controller, and the liquid distribution device includes a mobile phase A storage tank 1, a mobile phase B storage tank 2, and a mixing tank 3 , liquid addition tank 4, the mobile phase A storage tank 1 and the mobile phase B storage tank 2 are all connected to the mixing tank 3, and a flow control valve A6 is arranged between the mobile phase A storage tank 1 and the mixing tank 3 , a flow control valve B7 is arranged between the mobile phase B storage tank 2 and the mixing tank 3, a stirring device 8 is arranged in the mixing tank 3, and the liquid addition tank 4 is arranged below the mixing tank 3 , the liquid addition tank 4 is provided with a liquid concentration sensor 9, and the controller is electrically connected to the liquid concentration sensor 9, the flow control valve A6 and the flow control valve B7; the liquid addition tank 4 and the chromatographic column 5 Liquid is added through a delivery pump, and the chromatography column 5 includes a liquid inlet, a column body and a liquid outlet, and a liquid flow distributor 10 is arranged below the liquid inlet.
所述的加液罐4中设置有报警装置,所述的报警装置包括设置在加液罐4内的液位传感器11和设置在加液罐4外的报警器,所述的液位传感器11和报警器也与所述的控制器电连接。The described filling tank 4 is provided with an alarm device, and the described warning device comprises a liquid level sensor 11 arranged in the liquid adding tank 4 and an alarm device arranged outside the liquid adding tank 4, and the described liquid level sensor 11 And the alarm is also electrically connected with the controller.
所述的控制器为PLC控制器。Described controller is PLC controller.
所述的液流分布器10为喷雾式液流分布器。The liquid flow distributor 10 is a spray type liquid flow distributor.
所述的层析柱5的柱体的填料为硅胶或大孔吸附树脂。The packing of the column body of the chromatography column 5 is silica gel or macroporous adsorption resin.
所述的层析柱5的柱体为不锈钢柱体,且所述的柱体上设置有可视窗。The column body of the chromatography column 5 is a stainless steel column body, and the column body is provided with a viewing window.
所述的层析柱5的柱体外设置有温控夹套。A temperature control jacket is arranged outside the column of the chromatography column 5 .
所述的层析柱5的出液口连接有2~8个接液罐。The liquid outlet of the chromatography column 5 is connected with 2 to 8 liquid receiving tanks.
所述的接液罐均连接至离心式刮板薄膜浓缩器。The liquid receiving tanks are all connected to the centrifugal scraper film concentrator.
所述的输送泵为工业蠕动泵。The delivery pump is an industrial peristaltic pump.
本实用新型工作原理和工作过程:当大麻二酚粗提物样品装柱吸附结束后,先通过控制器调节流量控制阀A6和流量控制阀B7,使用流动相A(在大麻二酚的层析过程中采用纯化水)冲洗层析柱5一段时间,接着开始进行洗脱,先通过控制器调节流量控制阀A6和流量控制阀B7,将流动相A储罐1和流动相B储罐2中的流动相加入到混合罐3中,并将流动相A(大麻二酚的层析过程中为纯化水)和流动相B(大麻二酚的层析过程中为乙醇)通过搅拌装置8进行充分混合得到浓度均一的洗脱液,充分混合之后的洗脱液进入加液罐4,通过液体浓度传感器9检测液体浓度,并反馈到控制器,实时控制流量控制阀A6和流量控制阀B7使得加液罐4中的洗脱液配比稳定;而且,本实用新型也能够根据层析进程随时调整洗脱液的配比;通过在层析柱5的进液口下方设置液流分布器10,使得洗脱液分布均匀,操作稳定,有效提高分离效率。The working principle and working process of the utility model: after the column adsorption of the cannabidiol crude extract sample is completed, the flow control valve A6 and the flow control valve B7 are first adjusted by the controller, and the mobile phase A (in the chromatography of the cannabidiol Purified water (purified water) is used in the process to wash the chromatography column 5 for a period of time, and then the elution starts. First, the flow control valve A6 and the flow control valve B7 are adjusted by the controller, and the mobile phase A storage tank 1 and the mobile phase B storage tank 2 The mobile phase is added into the mixing tank 3, and the mobile phase A (purified water in the chromatography process of cannabidiol) and mobile phase B (ethanol in the chromatography process of cannabidiol) are fully mixed by the stirring device 8 Mix to obtain an eluent with uniform concentration, and the fully mixed eluent enters the liquid addition tank 4, detects the liquid concentration through the liquid concentration sensor 9, and feeds back to the controller to control the flow control valve A6 and flow control valve B7 in real time to make the addition The ratio of the eluent in the liquid tank 4 is stable; moreover, the utility model can also adjust the ratio of the eluent at any time according to the chromatography process; by setting the liquid flow distributor 10 under the liquid inlet of the chromatography column 5, The eluent is evenly distributed, the operation is stable, and the separation efficiency is effectively improved.
进一步的,当层析过程中液位传感器11的信号低于预设值时,控制器控制报警器进行报警,避免干柱现象,有效提高过柱的成功率,便于产物的分离。Further, when the signal of the liquid level sensor 11 is lower than the preset value during the chromatography process, the controller controls the alarm to give an alarm, so as to avoid the dry column phenomenon, effectively improve the success rate of passing through the column, and facilitate the separation of products.
进一步的,本实用新型可以选择PLC控制器。Further, the utility model can choose a PLC controller.
进一步的,本实用新型采用多个接液罐循环进行接液,当使用单一流动相(如纯化水)冲柱时,直接接液后不再进行处理,简化工艺,降低成本;而且多个接液罐分开接液,大大降低分离后的高纯度大麻二酚与杂质复混的可能性,有效提高分离效率,便于直接得到高纯度的产物。Further, the utility model adopts a plurality of liquid receiving tanks to receive liquid in a cycle. When a single mobile phase (such as purified water) is used to flush the column, no further treatment will be performed after directly contacting the liquid, which simplifies the process and reduces the cost; and multiple receiving tanks The liquid tank is separated from the liquid, which greatly reduces the possibility of the separated high-purity cannabidiol being mixed with impurities, effectively improves the separation efficiency, and facilitates the direct obtaining of high-purity products.
进一步的,层析柱5的柱体为不锈钢柱体,且柱体上设置有可视窗;不锈钢柱体能够适应工业生产的需要,同时可视窗的存在便于实时观察柱体的情况,避免柱体内填料出现气泡、断层等情况时无法及时发现和调整。Further, the column body of the chromatography column 5 is a stainless steel column body, and the column body is provided with a visual window; the stainless steel column body can meet the needs of industrial production, and the presence of the visual window facilitates real-time observation of the column body, avoiding Bubbles, faults, etc. in the filler cannot be detected and adjusted in time.
本实用新型操作简单,实现自动化,也大大减少了人工成本。The utility model has simple operation, realizes automation, and greatly reduces labor costs.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN111729351A (en) * | 2020-07-29 | 2020-10-02 | 辽宁石化职业技术学院 | Novel automatic chromatographic separation purification device |
US11040932B2 (en) | 2018-10-10 | 2021-06-22 | Treehouse Biotech, Inc. | Synthesis of cannabigerol |
US11084770B2 (en) | 2016-12-07 | 2021-08-10 | Treehouse Biotech, Inc. | Cannabis extracts |
US11202771B2 (en) | 2018-01-31 | 2021-12-21 | Treehouse Biotech, Inc. | Hemp powder |
-
2017
- 2017-10-26 CN CN201721392444.XU patent/CN207384906U/en active Active
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US11084770B2 (en) | 2016-12-07 | 2021-08-10 | Treehouse Biotech, Inc. | Cannabis extracts |
US11202771B2 (en) | 2018-01-31 | 2021-12-21 | Treehouse Biotech, Inc. | Hemp powder |
US11040932B2 (en) | 2018-10-10 | 2021-06-22 | Treehouse Biotech, Inc. | Synthesis of cannabigerol |
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 |
CN111729351A (en) * | 2020-07-29 | 2020-10-02 | 辽宁石化职业技术学院 | Novel automatic chromatographic separation purification device |
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Assignee: Yunnan Hanmeng Pharmaceutical Co., Ltd Assignor: Yunnan Hansu bio-technology Co.,Ltd. Contract record no.: X2020980001712 Denomination of utility model: A chromatographic device for draw cannabidiol among industrial hemp Granted publication date: 20180522 License type: Common License Record date: 20200423 |
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