阅读说明：本技术 一种超临界二氧化碳萃取装置及其方法 (A kind of supercritical carbon dioxide extraction apparatus and its method ) 是由 杨景峰 于 2019-09-26 设计创作，主要内容包括：本发明公开了一种超临界二氧化碳萃取装置及其方法,该萃取装置包括：一萃取釜；一与萃取釜底部连通的二氧化碳储罐；一通过管道分别与萃取釜顶部和二氧化碳储罐连通的分离釜；以及一通过管道与二氧化碳储罐连通的高压气罐；二氧化碳储罐内回收的液态或超临界二氧化碳,在高压空气持续增压的作用下,被输送至萃取釜内进行循环利用。本发明提供的超临界二氧化碳萃取装置及其方法,采用高压气体作为动力,快速调节各工艺流程段的超临界二氧化碳的压力,从而快速调节萃取釜内的超临界二氧化碳的溶解度,实现高效率萃取,且其具有工艺调整快、工艺稳定性高、控制精度高以及萃取效率高等优点。(The invention discloses a kind of supercritical carbon dioxide extraction apparatus and its method, which includes: an extraction kettle；One carbon dioxide storage tank being connected to extraction kettle bottom；One separating still being connected to respectively with extraction kettle top and carbon dioxide storage tank by pipeline；And the high pressure gas holder that is connected to carbon dioxide storage tank by pipeline；The liquid or supercritical carbon dioxide recycled in carbon dioxide storage tank is transported in extraction kettle and is recycled under the action of pressure-air is persistently pressurized.Supercritical carbon dioxide extraction apparatus provided by the invention and its method, using high pressure gas as power, quickly adjust the pressure of the supercritical carbon dioxide of each process flow section, to quickly adjust the solubility of the supercritical carbon dioxide in extraction kettle, realize high efficiency extraction, and it has many advantages, such as that technique adjustment is fast, technology stability is high, control precision is high and extraction efficiency is high.)

1. a kind of supercritical carbon dioxide extraction apparatus characterized by comprising

One is filled with the extraction kettle (15) of material to be extracted；

One carbon dioxide storage tank (8) being connected to by pipeline with the extraction kettle (15) bottom is used to be pressurized in pressure-air Under the action of to the extraction kettle (15) convey liquid or supercritical carbon dioxide, to dissolve respective sets in the extraction material Point；

One separating still (22) being connected to respectively with the extraction kettle (15) top and the carbon dioxide storage tank (8) by pipeline, It is used to receive the carbon dioxide mixture assembled at the top of the extraction kettle (15), and carries out gas to the carbon dioxide mixture Liquid separation, the carbon dioxide gas after separation pass through in pipeline to the carbon dioxide storage tank (8)；And

One high pressure gas holder (4) being connected to by pipeline with the carbon dioxide storage tank (8), is used for as the carbon dioxide storage tank (8) carbon dioxide recycled in provides the pressure-air of pressurization, conveying and/or phase change transition；

Wherein, the liquid or supercritical carbon dioxide recycled in the carbon dioxide storage tank (8), persistently increases in the pressure-air Under the action of pressure, it is transported in the extraction kettle (15) and is recycled.

2. supercritical carbon dioxide extraction apparatus according to claim 1, which is characterized in that further include:

One is installed in the second booster pump between the carbon dioxide storage tank (8) and the extraction kettle (15) bottom on pipeline (11)；And/or

One is installed in the heat exchanger (12) between the carbon dioxide storage tank (8) and the extraction kettle (15) bottom on pipeline.

3. supercritical carbon dioxide extraction apparatus according to claim 1, which is characterized in that further include:

One is installed in the forecooler (27) between the separating still (22) and the carbon dioxide storage tank (8) on pipeline, is used for Carbon dioxide gas after the separating still (22) separation is cooled down to liquid carbon dioxide.

4. supercritical carbon dioxide extraction apparatus according to claim 1, which is characterized in that the high pressure gas holder (4), two Thermocouple and pressure gauge are installed on carbonoxide storage tank (8), extraction kettle (15) and the separating still (22).

5. supercritical carbon dioxide extraction apparatus according to claim 1, which is characterized in that further include:

One the first booster pump (1) being connect by pipeline with the high pressure gas holder (4), is used to adjust the high pressure gas holder (4) Interior gas pressure.

6. supercritical carbon dioxide extraction apparatus according to claim 1, which is characterized in that in the high pressure gas holder (4) High pressure gas be air or inert gas.

7. supercritical carbon dioxide extraction apparatus according to claim 1, which is characterized in that extraction kettle (15) bottom It is installed with velocity flow profile device (14) comprising air inlet pipe (24) and the gas tank (25) with middle chamber, the gas tank (25) Top is evenly equipped with spray-hole (26), and the spray-hole (26) is connected to by the air inlet pipe (24) with the high pressure gas holder (4).

8. a kind of supercritical carbon dioxide extraction apparatus method of any one of such as claim 1-6 described device, which is characterized in that Include the following steps:

(1) supercritical carbon dioxide is uniformly spurted into extraction kettle from the bottom of extraction kettle, supercritical carbon dioxide is from bottom to top Flowing comes into full contact with extraction material, and selective dissolution needs the solute extracted；

(2) carbon dioxide mixture gathered at the top of extraction kettle is sent into after being depressured separating still and carries out gas-liquid separation, solute is heavy Product is sent into carbon dioxide storage tank in separating still bottom, carbon dioxide solvent from the top of separating still；

(3) high pressure gas is passed through into carbon dioxide storage tank from high pressure gas holder, will recycle under the pressurization of high pressure gas Carbon dioxide phase change transition be liquid or above-critical state, and be stored in carbon dioxide storage tank；

(4) continue to be passed through high pressure gas into carbon dioxide storage tank, the liquid recycled in carbon dioxide storage tank or overcritical dioxy Change carbon under the action of pressure-air is persistently pressurized, is transported in extraction kettle as extractant；

(5) repeat the above steps (1)-(4), realizes recycling for supercritical extract carbon dioxide in process.

9. supercritical carbon dioxide method for extracting according to claim 8, which is characterized in that dioxy described in step (2) Change after carbon solvent goes out at the top of separating still after condenser is cooled to liquid point temperature, in feeding carbon dioxide storage tank.

10. supercritical carbon dioxide method for extracting according to claim 8, which is characterized in that from described two in step (4) The liquid or supercritical carbon dioxide of carbonoxide storage tank discharge are successively pressurized through the second booster pump again, heat exchanger is warming up to super face After boundary's carbon dioxide, it is sent into extraction kettle and is used as extractant.

Technical field

The present invention relates to supercritical carbon dioxide extraction method fields more particularly to a kind of supercritical carbon dioxide extracting to fill It sets and its method.

Background technique

Traditional extraction process often results in the destruction of certain heat sensitive components or chemically unstable ingredient in natural products, from And change the peculiar flavour of natural products.Moreover, being also inevitable due to dissolvent residual at pollution in process.It is super Critical carbon dioxide abstraction technique has pure, safety, keeps that bioactivity, stability is strong, recovery rate is high etc. a little, becomes day A kind of new abstraction technique with development prospect in right object extraction.

However, existing supercritical carbon dioxide extracting has some disadvantages: that extraction process carries out under high pressure, extraction process Compressor, condenser and heat exchanger etc. are needed, the investment of equipment is high, and energy consumption is high.Supercritical carbon dioxide is in Near The Critical Point object Violent variation occurs with the minor change of temperature and pressure for property parameter, what the density with temperature of especially supercritical carbon dioxide wanted Change dramatically will lead to the solubility with temperature and pressure change dramatically of supercritical carbon dioxide, although this is conducive to improve extraction Efficiency and rate are taken, but will cause technological parameter and be difficult to control, the problem of technology stability difference.Existing abstraction technique extraction kettle It cannot operate continuously, the problems such as noise production efficiency and inefficiency.

Therefore, a kind of extract and separation process operation process temperature near room temperature, reduction compressor and Re Jiao how is developed The supercritical carbon dioxide extraction that capacity, the technique adjustment of parallel operation are fast, technology stability is high, control precision is high and extraction efficiency is high Taking technology is those skilled in the art's technical problem urgently to be resolved.

Summary of the invention

To be solved by this invention and problem in view of the above-mentioned drawbacks in the prior art, proposes a kind of supercritical carbon dioxide The operation process temperature near room temperature of extraction equipment and its method, the supercritical carbon dioxide extraction apparatus and its method reduces The capacity of compressor and heat exchanger, and have that technique adjustment is fast, technology stability is high, control precision is high and extraction efficiency The advantages that high.

To achieve the above object, the invention adopts the following technical scheme:

The first aspect of the invention is to provide a kind of supercritical carbon dioxide extraction apparatus, specifically includes that

One is filled with the extraction kettle of material to be extracted；

One carbon dioxide storage tank being connected to by pipeline with the extraction kettle bottom, is used for the work being pressurized in pressure-air Liquid or supercritical carbon dioxide are conveyed to the extraction kettle with lower, to dissolve respective components in the extraction material；

One separating still being connected to respectively with the extraction kettle top and the carbon dioxide storage tank by pipeline, is used to connect The carbon dioxide mixture assembled at the top of the extraction kettle is received, and gas-liquid separation, separation are carried out to the carbon dioxide mixture Carbon dioxide gas afterwards passes through in pipeline to the carbon dioxide storage tank；And

One high pressure gas holder being connected to by pipeline with the carbon dioxide storage tank, is used for as in the carbon dioxide storage tank The carbon dioxide of recycling provides the pressure-air of pressurization, conveying and/or phase change transition；

Wherein, the liquid or supercritical carbon dioxide recycled in the carbon dioxide storage tank continues in the pressure-air Under the action of pressurization, it is transported in the extraction kettle and is recycled.

Further, on the supercritical carbon dioxide extraction apparatus, further includes:

One is installed in the second booster pump between the carbon dioxide storage tank and the extraction kettle bottom on pipeline；And/or

One is installed in the heat exchanger between the carbon dioxide storage tank and the extraction kettle bottom on pipeline.

It is further preferred that on the supercritical carbon dioxide extraction apparatus, further includes:

One is installed in the first mass flowmenter on the pipeline between the carbon dioxide storage tank and second booster pump；

One is installed in the second mass flowmenter between the heat exchanger and the extraction kettle bottom on pipeline；And

One is installed in the third mass flowmenter between the extraction kettle and the separating still on pipeline.

Further, on the overcritical extraction carbon dioxide extraction apparatus, further includes:

One is installed in the forecooler between the separating still and the carbon dioxide storage tank on pipeline, is used for described point It cools down from the carbon dioxide gas after kettle separation to liquid carbon dioxide.

Further, on the supercritical carbon dioxide extraction apparatus, the high pressure gas holder, carbon dioxide storage tank, Regulating valve is installed on the pipeline connected between extraction kettle and the separating still.

Further, on the supercritical carbon dioxide extraction apparatus, the high pressure gas holder, carbon dioxide storage tank, Thermocouple and pressure gauge are installed on extraction kettle and the separating still.

Further, on the supercritical carbon dioxide extraction apparatus, further includes:

One, by pipeline and tank connected first booster pump of the high pressure gas, is used to adjust the gas in the high pressure gas holder Body pressure.

Further, on the supercritical carbon dioxide extraction apparatus, the high pressure gas in the high pressure gas holder is Air or inert gas.

Further, on the supercritical carbon dioxide extraction apparatus, the extraction kettle bottom is installed with flow velocity point Cloth device comprising air inlet pipe and the gas tank with middle chamber are evenly equipped with spray-hole at the top of the gas tank, and the spray-hole is logical The air inlet pipe is crossed to be connected to the high pressure gas holder.

The second aspect of the invention is to provide a kind of supercritical carbon dioxide method for extracting such as described device, including such as Lower step:

(1) supercritical carbon dioxide is uniformly spurted into extraction kettle from the bottom of extraction kettle, supercritical carbon dioxide is under It flows up and is come into full contact with extraction material, selective dissolution needs the solute extracted；

(2) carbon dioxide mixture gathered at the top of extraction kettle is sent into after being depressured separating still and carries out gas-liquid separation, it is molten Matter is deposited on separating still bottom, and carbon dioxide solvent is sent into carbon dioxide storage tank from the top of separating still；

(3) high pressure gas is passed through into carbon dioxide storage tank from high pressure gas holder, to incite somebody to action under the pressurization of high pressure gas The carbon dioxide phase change transition of recycling is liquid or above-critical state, and is stored in carbon dioxide storage tank；

(4) continue to be passed through high pressure gas into carbon dioxide storage tank, the liquid or overcritical recycled in carbon dioxide storage tank Carbon dioxide is transported in extraction kettle under the action of pressure-air is persistently pressurized as extractant；

(5) repeat the above steps (1)-(4), realizes recycling for supercritical extract carbon dioxide in process.

Further, in the overcritical extraction carbon dioxide method for extracting, carbon dioxide solvent described in step (2) goes out After at the top of separating still after condenser is cooled to liquid point temperature, it is sent into carbon dioxide storage tank.

Further, it in the supercritical carbon dioxide method for extracting, is arranged in step (4) from the carbon dioxide storage tank Liquid out or supercritical carbon dioxide is successively pressurized through the second booster pump again, heat exchanger is warming up to supercritical carbon dioxide Afterwards, it is sent into extraction kettle and is used as extractant.

The present invention by adopting the above technical scheme, compared with prior art, has the following technical effect that

(1) use supercritical carbon dioxide for extractant, go have extracting power more stronger than conventional extraction process and Recovery rate can be increased to by adjusting optimised process close to 100% by higher extraction yield；And supercritical carbon dioxide Critical-temperature not only contributes to operate close to room temperature, and the effective component that can effectively save extract is not destroyed；

(2) simultaneously as the critical point of carbon dioxide is close to room temperature, therefore compressor and heat be can reduce in extraction process The capacity of exchanger improves the stability of extraction process；

(3) power is used as using high pressure gas (inert gas or air), can quickly adjusted overcritical in extraction kettle The pressure (in one timing of technique object temperature) of carbon dioxide, to quickly adjust the solubility of supercritical carbon dioxide, is realized high Efficiency extraction；

(4) compared with conventional supercritical fluid CO 2 extraction technology, using high pressure gas to being recycled in carbon dioxide storage tank Carbon dioxide carry out pressure adjusting, complete transformation of the carbon dioxide from gaseous state to liquid or above-critical state, tradition be omitted Transformation of the carbon dioxide realized in carbon dioxide recovery technique using supercharging equipment and condenser from gaseous state to liquid, is reduced The investment of compressor and condenser；

(5) pressure adjusting is carried out to the carbon dioxide recycled in carbon dioxide storage tank using high pressure gas, makes the two of recycling Carbonoxide is changed from gaseous state to liquid or above-critical state, and the liquid or the supercritical carbon dioxide of recycling are passed through extraction kettle ginseng again With extraction, the recycling of carbon dioxide abstraction solvent is realized, reduces the dosage of supercritical carbon dioxide；

(6) by the way that the velocity flow profile device of specific structure is arranged in extraction kettle bottom, divide carbon dioxide uniformly from bottom to top Cloth shortens extraction time to increase two-phase respectively specific surface area, improves extracting power；

(7) supercritical carbon dioxide extraction apparatus, have technique adjustment is fast, technology stability is high, control precision height with And extraction efficiency it is high the advantages that, and its structure is simple, and easy to operate, low energy consumption, reduces labor intensity, reduce operation at This.

Detailed description of the invention

Fig. 1 is a kind of structural schematic diagram of supercritical carbon dioxide extraction apparatus of the present invention；

Fig. 2 is the side structure schematic view of velocity flow profile device in a kind of supercritical carbon dioxide extraction apparatus of the present invention；

Fig. 3 is the overlooking structure diagram of velocity flow profile device in a kind of supercritical carbon dioxide extraction apparatus of the present invention；

Wherein, each appended drawing reference are as follows:

The first booster pump of 1-, the first thermocouple of 2-, 3- first pressure gauge, 4- high pressure gas holder, the first regulating valve of 5-, 6- second Thermocouple, 7- second pressure gauge, 8- carbon dioxide storage tank, the first mass flowmenter of 9-, the second regulating valve of 10-, 11- second are pressurized Pump, 12- heat exchanger, the second mass flowmenter of 13-, 14- velocity flow profile device, 15- extraction kettle, 16- third pressure gauge, 17- third Thermocouple, 18- third regulating valve, 19- third mass flowmenter, the 4th pressure gauge of 20-, the 4th thermocouple of 21-, 22- separating still, The 4th regulating valve of 23-, 24- air inlet pipe, 25- gas tank, 26- spray-hole.

Specific embodiment

The present invention is described in more detail below by specific embodiment, for a better understanding of the present invention, But following embodiments are not intended to limit the scope of the invention.