阅读说明：本技术 超临界萃取-分子蒸馏联用装置 (Supercritical extraction-molecular distillation combined device ) 是由 许杨 傅尧 徐清 于 2020-06-02 设计创作，主要内容包括：本发明公开了一种超临界萃取-分子蒸馏联用装置包括超临界萃取单元和分子蒸馏单元,所述超临界萃取单元与所述分子蒸馏单元管道连接,所述超临界萃取-分子蒸馏联用装置具有结构紧凑,操作简单的特点,精简了超临界萃取-分子蒸馏装置的体积,简化了超临界萃取-分子蒸馏的工艺衔接操作。(The invention discloses a supercritical extraction-molecular distillation combined device which comprises a supercritical extraction unit and a molecular distillation unit, wherein the supercritical extraction unit is connected with the molecular distillation unit through a pipeline, and the supercritical extraction-molecular distillation combined device has the characteristics of compact structure and simplicity in operation, so that the volume of the supercritical extraction-molecular distillation device is reduced, and the process connection operation of the supercritical extraction-molecular distillation is simplified.)

1. A combined supercritical extraction and molecular distillation apparatus, comprising:

the device comprises a supercritical extraction unit and a molecular distillation unit, wherein the supercritical extraction unit is connected with the molecular distillation unit through a pipeline.

2. The combined supercritical extraction-molecular distillation apparatus according to claim 1, wherein the supercritical extraction unit comprises a gas cylinder, an extraction condenser, an entrainer bottle, an extraction kettle and a separation kettle which are connected by pipelines in sequence.

3. The combined supercritical extraction-molecular distillation apparatus according to claim 2, wherein the extraction kettle comprises one monomer extraction kettle, or the extraction kettle comprises a plurality of monomer extraction kettles, and the plurality of monomer extraction kettles are connected in series or in parallel.

4. The combined supercritical extraction-molecular distillation apparatus according to claim 2, wherein the separation vessel comprises one monomer separation vessel, or the separation vessel comprises a plurality of monomer separation vessels, and the plurality of monomer separation vessels are connected in series or in parallel.

5. The combined supercritical extraction and molecular distillation apparatus according to claim 1, wherein the molecular distillation unit comprises a cylinder, and the inner wall of the cylinder is provided with a molecular distillation heating surface;

the top of the cylinder body is provided with a fixedly installed motor, and a rotating shaft of the motor is inserted into the cylinder body;

the bottom of the rotating shaft is fixedly connected with a molecular distillation film scraper, wherein the molecular distillation film scraper is tightly attached to the molecular distillation heating surface;

a distillation condenser is arranged in the inner cavity of the cylinder body and fixed at the bottom of the cylinder body;

the bottom of the cylinder body is provided with an outlet, and the outlet is connected with a collecting bottle pipeline.

6. The combined supercritical extraction and molecular distillation apparatus according to claim 5 wherein the outlet comprises a first outlet and a second outlet, the collection bottle comprises a light fraction collection bottle connection and a heavy fraction collection bottle, wherein the first outlet is connected to the light fraction collection bottle by a conduit, and the second outlet is connected to the heavy fraction collection bottle by a conduit.

7. The combined supercritical extraction and molecular distillation apparatus of claim 5 wherein the molecular distillation heating surface comprises one of a jacketed glass type molecular distillation heating surface, an electrically heated wire type molecular distillation heating surface;

the molecular distillation heating surface is made of metal or glass.

8. The combined supercritical extraction and molecular distillation apparatus according to claim 5 wherein the distillation condenser is a liquid cooled condenser or a semiconductor refrigerated condenser.

9. The combined supercritical extraction and molecular distillation apparatus according to claim 5, wherein the molecular distillation scraper is a roller molecular distillation scraper or a scraper molecular distillation scraper.

10. The combined supercritical extraction-molecular distillation apparatus according to claim 5 or 6, wherein the bottom of the cylinder is further provided with a third outlet, and the third outlet is connected with a vacuum pump pipeline.

Technical Field

The invention relates to the technical field of extraction and separation, in particular to a supercritical extraction-molecular distillation combined device.

Background

In the fields of food, medicine, fine chemical engineering and the like, the extraction and separation of substances are often required to be carried out by means of supercritical extraction and molecular distillation simultaneously. Generally, the product obtained by supercritical extraction contains more components and impurities, and needs to be further separated and purified by molecular distillation.

However, currently there is only a single supercritical extraction unit and a single molecular distillation unit. If the product of supercritical extraction needs to be subjected to molecular distillation, an operator needs to put the product of supercritical extraction into the molecular distillation device again, so that two devices with huge volumes are needed, the occupied area is large, and the process connection is complex.

Disclosure of Invention

The invention provides a supercritical extraction-molecular distillation combined device, aiming at simplifying the volume of the device and simplifying the process connection operation of the supercritical extraction-molecular distillation.

In order to achieve the above object, the present invention provides a combined supercritical extraction and molecular distillation apparatus, comprising:

the device comprises a supercritical extraction unit and a molecular distillation unit, wherein the supercritical extraction unit is connected with the molecular distillation unit through a pipeline.

Preferably, the supercritical extraction unit comprises a gas cylinder, an extraction condenser, an entrainer bottle, an extraction kettle and a separation kettle which are sequentially connected through pipelines.

Preferably, the extraction kettle comprises one monomer extraction kettle, or the extraction kettle comprises a plurality of monomer extraction kettles, and the plurality of monomer extraction kettles are connected in series or in parallel.

Preferably, the separation kettle comprises one monomer separation kettle, or the separation kettle comprises a plurality of monomer separation kettles, and the plurality of monomer separation kettles are connected in series or in parallel.

Preferably, the molecular distillation unit comprises a cylinder, and the inner wall of the cylinder is provided with a molecular distillation heating surface;

the top of the cylinder body is provided with a fixedly installed motor, and a rotating shaft of the motor is inserted into the cylinder body;

the bottom of the rotating shaft is fixedly connected with a molecular distillation film scraper, wherein the molecular distillation film scraper is tightly attached to the molecular distillation heating surface;

a distillation condenser is arranged in the inner cavity of the cylinder body and fixed at the bottom of the cylinder body;

the bottom of the cylinder body is provided with an outlet, and the outlet is connected with a collecting bottle pipeline.

Preferably, the outlet comprises a first outlet and a second outlet, and the collecting bottle comprises a light component collecting bottle connection and a heavy component collecting bottle, wherein the first outlet is connected with the light component collecting bottle through a pipeline, and the second outlet is connected with the heavy component collecting bottle through a pipeline.

Preferably, the molecular distillation heating surface comprises one of a jacket glass type molecular distillation heating surface and an electric heating wire type molecular distillation heating surface;

the molecular distillation heating surface is made of metal or glass.

Preferably, the distillation condenser is a liquid-cooled condenser or a semiconductor-cooled condenser.

Preferably, the molecular distillation scraper is a roller-type molecular distillation scraper or a scraper-type molecular distillation scraper.

Preferably, the bottom of the cylinder is further provided with a third outlet, and the third outlet is connected with a vacuum pump pipeline.

Compared with the prior art, the supercritical extraction-molecular distillation combined device provided by the invention comprises a supercritical extraction unit and a molecular distillation unit, wherein the supercritical extraction unit is connected with the molecular distillation unit through a pipeline, and the supercritical extraction-molecular distillation combined device has the characteristics of compact structure and simplicity in operation, so that the volume of the supercritical extraction-molecular distillation device is reduced, and the process connection operation of the supercritical extraction-molecular distillation is simplified.

Drawings

FIG. 1 is a schematic structural diagram of a combined supercritical extraction-molecular distillation apparatus according to the present invention.

The reference numbers illustrate:

reference numerals	Name (R)	Reference numerals	Name (R)
				1	Gas cylinder	9	Molecular distillation film scraper
2	Extraction condenser	10	Distillation condenser
				3	Entrainer bottle	11	Light component collecting bottle
4	Extraction kettle	12	Heavy component collecting bottle
				5	Separation kettle	13	Valve gate
6	Electric machine	14	Pump and method of operating the same
				7	Barrel body	15	CO2Pump and method of operating the same
8	Molecular distillation heating surface

The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.

Detailed Description

It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

The embodiment of the invention provides a supercritical extraction-molecular distillation combined device. The supercritical extraction-molecular distillation combined device comprises a supercritical extraction unit and a molecular distillation unit, wherein the supercritical extraction unit is connected with the molecular distillation unit through a pipeline.

The supercritical extraction unit is used for supercritical extraction. The density of the supercritical fluid CO2 is sensitive to temperature and pressure changes, and the dissolving capacity of the supercritical fluid CO2 for substances to be separated can be adjusted by adjusting the temperature and the pressure of the supercritical fluid CO 2. In the supercritical state, supercritical fluid CO2 is contacted with the substance to be separated, so that the components with polarity, boiling point and molecular weight are selectively extracted in turn. Of course, the extracts obtained corresponding to each pressure range cannot be single, but the conditions can be controlled to obtain the mixed components with the optimal proportion, then the supercritical fluid CO2 is changed into the common gas by the methods of pressure reduction and temperature rise, and the extracted substances are completely or basically precipitated, thereby achieving the purpose of separation and purification.

The molecular distillation unit is used for molecular distillation. Molecular distillation is a distillation process operating under vacuum, which uses the difference in the mean free path of motion of different species molecules to effect separation of species. When the liquid mixture to be separated flows along the heating plate and is heated, the light and heavy component molecules escape from the liquid surface into the gas phase. Because the free paths of the light component molecules and the heavy component molecules are different, the moving distances of the molecules of different components after escaping from the liquid surface are different, the condensing plate is arranged at a reasonable distance, when the light component molecules reach the condensing plate, the light component molecules are condensed into liquid, but the heavy component molecules cannot reach the condensing plate, and therefore the separation of the light component molecules and the heavy component molecules can be realized.

Specifically, referring to fig. 1, fig. 1 is a schematic structural diagram of a combined supercritical extraction and molecular distillation apparatus according to the present invention.

As shown in fig. 1, the supercritical extraction unit comprises a gas cylinder 1, an extraction condenser 2, an entrainer cylinder 3, an extraction kettle 4 and a separation kettle 5 which are connected in sequence through pipelines.

The gas cylinder 1 is connected with the extraction condenser 2 through a pipeline. Generally, the extractant in the gas cylinder 1 is liquefied after passing through the extraction condenser 2. The extraction condenser 2 is also connected with the entrainer bottle 3 through a pipeline and is connected to the extraction kettle 4, so that the liquefied extractant is mixed with the entrainer in the entrainer bottle 3 and then enters the extraction kettle 4, and the solution to be extracted in the extraction kettle 4 is extracted.

Further, the extraction kettle 4 is connected with the separation kettle 5 through a pipeline, after the extraction process is completed, the solution to be extracted, the extractant and the entrainer in the extraction kettle 4 enter the separation kettle 5 to be subjected to gas-liquid separation, the separated gas is discharged or recycled through a circulating pipeline, and the separated liquid extract enters the molecular distillation unit.

Further, the extraction kettle 4 comprises a monomer extraction kettle 4, or the extraction kettle 4 comprises a plurality of monomer extraction kettles 4, and the plurality of monomer extraction kettles 4 are connected in series or in parallel. Thus, multi-stage extraction can be realized based on the monomer extraction kettles 4 connected in series or in parallel.

Further, the separation kettle 5 comprises a monomer separation kettle 5, or the separation kettle 5 comprises a plurality of monomer separation kettles 5, and the monomer separation kettles 5 are connected in series or in parallel. Thus, multistage separation can be achieved based on the monomer separation vessels 5 in series or in parallel.

In addition, the supercritical extraction unit further comprises a plurality of valves 13, the valves 13 are respectively arranged on the gas cylinder 1 and the pipeline of the extraction condenser 2, the extraction condenser 2 and the pipeline of the extraction kettle 4, the entrainer bottle 3 and the pipeline of the extraction kettle 4, the extraction kettle 4 and the pipeline of the separation kettle 5, and the extraction condenser 2 and the pipeline of the separation kettle 5.

Further, a pipeline connecting the extraction condenser 2 and the separation kettle 5 is also provided with CO₂Pump 15, said CO₂The pump 15 is used for extracting CO in the separation kettle 5₂Pumping gas into the extraction condenser 2 to realize CO₂The recycling of (2).

In addition, the extraction condenser 2 and the extraction kettle 4 are also provided with a pump 14 on the pipeline, and the entrainer bottle 3 and the extraction kettle 4 are also provided with a pump 14 on the pipeline.

The supercritical extraction unit is connected with the molecular distillation unit through a pipeline, and specifically, the supercritical extraction unit is connected with a barrel 7 in the molecular distillation unit through a separation kettle 5 in the supercritical extraction unit. And a valve 13 and a pump 14 are arranged on a pipeline connecting the separation kettle 5 and the cylinder 7, so that the separated liquid extract is pumped 14 into the molecular distillation unit.

With continued reference to fig. 1, the molecular distillation unit comprises a cylinder 7, and the inner wall of the cylinder 7 is provided with a molecular distillation heating surface 8; generally, the cylinder 7 is cylindrical. The molecular distillation heating surface 8 comprises a jacket glass type molecular distillation heating surface and an electric heating wire type molecular distillation heating surface; the molecular distillation heating surface 8 is made of metal or glass.

A motor is fixedly installed at the top of the cylinder 7, and a rotating shaft of the motor is inserted into the cylinder 7; the bottom of the rotating shaft is fixedly connected with a molecular distillation film scraper 9, wherein the molecular distillation film scraper 9 is tightly attached to the molecular distillation heating surface 8; the motor drives the molecular distillation film scraper 9 to rotate. The molecular distillation film scraper 9 is a roller type molecular distillation film scraper 9 or a scraper type molecular distillation film scraper 9. A distillation condenser 10 is arranged in the inner cavity of the cylinder 7, and the distillation condenser 10 is fixed at the bottom of the cylinder 7; the distillation condenser 10 is a liquid-cooled condenser or a semiconductor-cooled condenser

The bottom of the cylinder body 7 is provided with an outlet which is connected with a collecting bottle pipeline. The outlet comprises a first outlet and a second outlet, the collecting bottle comprises a light component collecting bottle 11 and a heavy component collecting bottle 12, the first outlet is connected with the light component collecting bottle 11 through a pipeline, and the second outlet is connected with the heavy component collecting bottle 12 through a pipeline.

And a third outlet is also arranged at the bottom of the cylinder body 7 and is connected with a vacuum pump pipeline. And vacuumizing the cylinder 7 by the vacuum pump to reach the vacuum degree required by molecular distillation.

In addition, a valve 13 is arranged on the pipeline of the barrel 7 and the light component collecting bottle 11 to control the light component to flow out of the barrel 7; the pipeline between the cylinder 7 and the heavy component collecting bottle 12 is also provided with a valve 13 for the heavy component to flow out of the cylinder 7.

After the separated liquid extract enters the molecular distillation unit, the liquid extract flows into the molecular distillation heating surface 8, is uniformly coated on the molecular distillation heating surface 8 by the molecular distillation film scraper 9, and is heated by the molecular distillation heating surface 8. After the liquid extract is heated, light and heavy component molecules in the liquid extract can escape from the liquid surface and enter a gas phase, part of the component molecules are captured by the distillation condenser 10 to obtain light components, and part of the component molecules stay on the molecular distillation heating surface 8 to become heavy components, wherein the light components flow out from the first outlet and enter the light component collecting bottle 11, and the heavy components flow out from the second outlet and enter the heavy component collecting bottle 12. Thereby realizing the separation of light and heavy components.

Generally, if the liquid extract of supercritical extraction needs to be further subjected to molecular distillation, experimenters are required to transfer the liquid extract to a molecular distillation device, the process needs manual operation of the experimenters, and the liquid extract is exposed to air during the transfer to the molecular distillation device, which may cause components in the liquid extract to be oxidized. However, in this embodiment, the combined supercritical extraction and molecular distillation apparatus eliminates the step of transferring the liquid extract to the molecular distillation apparatus by an experimenter, and ensures that the components in the liquid extract are not oxidized.

According to the scheme, the supercritical extraction-molecular distillation combined device comprises a supercritical extraction unit and a molecular distillation unit, wherein the supercritical extraction unit is connected with the molecular distillation unit through a pipeline, and the supercritical extraction-molecular distillation combined device has the characteristics of compact structure and simplicity in operation, so that the volume of the supercritical extraction-molecular distillation device is reduced, and the process connection operation of the supercritical extraction-molecular distillation is simplified.

It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or system that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or system. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, article, or system that comprises the element.

The above-mentioned serial numbers of the embodiments of the present invention are merely for description and do not represent the merits of the embodiments.

Through the above description of the embodiments, those skilled in the art will clearly understand that the method of the above embodiments can be implemented by software plus a necessary general hardware platform, and certainly can also be implemented by hardware, but in many cases, the former is a better implementation manner. Based on such understanding, the technical solution of the present invention may be embodied in the form of a software product, which is stored in a storage medium (e.g., ROM/RAM, magnetic disk, optical disk) as described above and includes instructions for causing a terminal device to execute the method according to the embodiments of the present invention.

The above description is only for the preferred embodiment of the present invention and is not intended to limit the scope of the present invention, and all equivalent structures or flow transformations made by the present specification and drawings, or applied directly or indirectly to other related arts, are included in the scope of the present invention.