A method for supercritical extraction of ganoderma lucidum spore oil without granulation

Abstract

The present invention relates to a method for supercritical extraction of ganoderma lucidum spore oil without granulation, which comprises the following steps: putting ganoderma lucidum spore powder raw material into a material basket, then putting the material basket into an extraction kettle, and sealing the extraction kettle; then 2 CO in the gas source 2 The high pressure pump is pumped into the extraction kettle, and the CO 2 The extracted Ganoderma lucidum spore oil and supercritical CO 2 The extracted spore oil is separated from the extractor by the separator. After the extraction is completed, the extracted spore oil is collected from the separator. The extractor is equipped with a supercritical CO 2 The guide plate of the fluid flow state makes the supercritical CO 2 The fluid passes through the fluid distributor at a steady speed and then contacts and transfers mass with the material in the material basket. Compared with the prior art, the present invention simplifies the supercritical CO 2 The extraction step reduces the production cost of Ganoderma lucidum spore oil.

Description

Technical Field

[0001] The invention relates to the field of ganoderma lucidum spore oil extraction technology, and in particular to a granulation-free supercritical extraction method for ganoderma lucidum spore oil. Background Art

[0002] Ganoderma lucidum is known as one of the nine immortal herbs. Ganoderma lucidum spore powder refers to the concentrated Ganoderma lucidum spores, which are in powder form. Ganoderma lucidum spores, commonly known as Ganoderma lucidum seeds, are the reproductive cells of Ganoderma lucidum. They are small particles produced from the cap during the growth and maturity of Ganoderma lucidum, and contain all the genetically active substances of Ganoderma lucidum. Ganoderma lucidum spore oil is an oily lipid extracted from Ganoderma lucidum spores, which contains rich triterpenoid substances and has a wide range of physiological activities. It can significantly improve the body's immunity, hypoxia tolerance and cholesterol reduction. Ganoderma lucidum spore oil also has significant anti-tumor and anti-radiation functions, prevents and treats cardiovascular diseases, regulates the nervous system, detoxifies and protects the liver. In recent years, Ganoderma lucidum spore oil products have become a treasure among health products with very important applications and economic value. Therefore, the preparation method and process technology of Ganoderma lucidum spore oil have become one of the hot topics of research. Because the main component of the cell wall of Ganoderma lucidum spores is chitin, which is very tough and dense, the extraction of Ganoderma lucidum spore oil from Ganoderma lucidum spores generally requires the Ganoderma lucidum spores to be pre-treated by breaking the cell wall, and the broken Ganoderma lucidum spore powder is used as the raw material for extraction. The extraction methods are mainly organic solvent extraction and supercritical CO2 extraction. Because CO2 is colorless, odorless, non-toxic, inert, and cheap, recently, the research results of extracting Ganoderma lucidum spore oil using supercritical CO2 have been reported one after another, and the method and process conditions for extracting Ganoderma lucidum spore oil using supercritical CO2 have been disclosed and authorized.

[0003] The applicant believes that, since the broken wall spore powder of Ganoderma lucidum is very fine, when using supercritical CO2 to extract Ganoderma lucidum spore oil, if the Ganoderma lucidum spore powder is not granulated in advance, when the supercritical CO2 fluid enters the material basket in the extraction kettle from the air inlet at the bottom of the extraction kettle and contacts the material, due to the high flow rate of supercritical CO2, it is easy to blow away the Ganoderma lucidum spore powder particles in the material basket to form a "channel flow" (also known as a "short circuit"). When this phenomenon occurs, CO2 will not contact the material, but directly pass through the channel of the "channel flow", so that CO2 does not play the role of extraction, or this part of CO2 does not extract the material; in addition, the high-speed supercritical CO2 may also squeeze some Ganoderma lucidum spore powder particles to the bottom of the upper baffle of the material basket to form a knot, blocking the air outlet, resulting in a decrease in extraction efficiency. Therefore, the total amount of Ganoderma lucidum spore oil extracted by unit CO2 is greatly reduced. In order to achieve the same extraction rate, it is necessary to increase the extraction time, thereby greatly reducing the extraction efficiency. Even in the case of severe "channel flow", even if the extraction time is extended, the extraction rate cannot be improved.

[0004] Therefore, at present, the articles and patents reported on supercritical CO2 extraction of Ganoderma lucidum spore oil basically involve raw material granulation or adding fillers such as glass balls and activated carbon materials to improve the extraction efficiency. The authorized invention patent [200610035574.8, Preparation method of whole Ganoderma lucidum spore oil] discloses that the Ganoderma lucidum spore oil is extracted by supercritical CO2 through pretreatment of broken Ganoderma lucidum spore powder granulation and using ethanol and ethyl acetate as carriers. The authorized invention patent [200610033686.X A method for extracting Ganoderma lucidum spore oil by supercritical CO2] discloses that the extraction mass transfer effect is improved by adding fillers such as stripping beads and activated carbon to the Ganoderma lucidum spore powder raw material, and the highest Ganoderma lucidum spore oil yield reaches 30%. The authorized invention patent [201310237869.3, a method for extracting Ganoderma lucidum spore oil using supercritical CO2 with variable temperature and pressure] provides a method for extracting Ganoderma lucidum spore oil by granulating Ganoderma lucidum spore powder through broken wall and using supercritical CO2 with 20-95% ethanol as a carrier, and Ganoderma lucidum spore oil with different proportions of components is obtained in different separators. The authorized patent [201010203684.7, a method for supercritical CO2 extraction and graded purification of Ganoderma lucidum spore oil] provides a method for extracting Ganoderma lucidum spore oil by pretreatment of broken Ganoderma lucidum spore powder granulation and multi-stage separation. The CO2 circulation amount required to process 1kg of Ganoderma lucidum spore powder raw material is 95kg; the patent under review [201620136746.4, a method for supercritical CO2 extraction of Ganoderma lucidum spore oil without granulation] aims at the problem that the extraction method of Ganoderma lucidum spore oil requires granulation, and proposes a method of placing a bag in the material hanging basket and then putting the raw materials into the bag to prevent "material leakage". However, although this method can prevent the "material leakage" of ungranulated Ganoderma lucidum spore powder, it cannot improve the problem of raw material agglomeration causing channeling and reducing mass transfer effect during supercritical CO2 extraction. The published patent [202110299381.8, a supercritical extraction process for Ganoderma lucidum spore oil with a high extraction rate] provides a step of combining steam explosion of Ganoderma lucidum spore powder with granulation, and uses supercritical CO2 to extract Ganoderma lucidum spore oil, thereby improving the extraction rate of active substances in triterpenes.

[0005] Although many patents have provided methods and process conditions for supercritical CO2 extraction of Ganoderma lucidum spore oil, the following problems still exist in the current supercritical CO2 extraction of Ganoderma lucidum spore oil: 1. All authorized patents involve the use of Ganoderma lucidum spore powder for granulation pretreatment and then supercritical CO2 extraction, which undoubtedly increases the equipment cost and processing cost of granulation pretreatment; 2. In the supercritical CO2 extraction process, some publicly authorized patent methods require the use of a method of adding a carrier; 3. The extraction time is long, and the amount of CO2 required to circulate per unit mass of Ganoderma lucidum spore oil is large. Therefore, these factors increase the production cost of Ganoderma lucidum spore oil. Summary of the invention

[0006] The purpose of the present invention is to overcome at least one of the defects of the above-mentioned prior art and to provide a granulation-free supercritical CO2 extraction method for Ganoderma lucidum spore oil, which simplifies the supercritical CO2 extraction steps, reduces the production cost of Ganoderma lucidum spore oil, and improves the yield of triterpenoid active ingredients. The method can not only significantly shorten the extraction time, thereby increasing the yield of Ganoderma lucidum spore oil per unit time, but also reduce the amount of CO2 required to circulate for extracting unit mass of Ganoderma lucidum spore oil, thereby improving the extraction efficiency and reducing the production cost of Ganoderma lucidum spore oil.

[0007] The purpose of the present invention can be achieved by the following technical solutions:

[0008] The present invention innovatively proposes to improve the mass transfer effect between supercritical CO2 and materials from another aspect, thereby improving the extraction efficiency and reducing the production cost. That is, the present invention designs and constructs a guide plate at the bottom of the extractor, and the guide plate can change the flow state of the supercritical CO2 fluid entering from the inlet of the extraction kettle, so that the supercritical CO2 can pass through the fluid distributor at the bottom of the material basket at a uniform speed and contact the material in the material basket for mass transfer, thereby improving the mass transfer effect. The present invention eliminates the raw material granulation pretreatment step, establishes the optimal combination conditions of extraction pressure, extraction temperature and CO2 flow rate, minimizes the CO2 circulation amount per unit mass of Ganoderma lucidum spore oil, and minimizes the extraction time, thereby improving the efficiency of extracting Ganoderma lucidum spore oil and reducing the production cost of Ganoderma lucidum spore oil. The method is simple, green, and easy to industrially scale up. The specific scheme is as follows:

[0009] A method for extracting ganoderma lucidum spore oil by supercritical extraction without granulation, the method comprising the following steps:

[0010] After the ganoderma lucidum spore powder raw material is loaded into the material basket, the material basket is then placed in the extraction kettle, and the extraction kettle is sealed; the extraction kettle is provided with a guide plate for changing the flow state of the supercritical CO2 fluid before entering the fluid distributor, so that the supercritical CO2 fluid passes through the fluid distributor at a uniform speed and contacts the material in the material basket for mass transfer; due to the effect of the guide plate, CO2 can pass through the fluid distributor at a uniform speed and enter the material basket for uniform mass transfer with the material, avoiding the formation of "channel flow" such as Figure 2 (b). In the subsequent comparative experiments, we further compared Figure 2 (a) with Figure 2 (b) Results.

[0011] The CO2 in the CO2 gas source is pumped into the extraction kettle through a high-pressure pump, and extraction is carried out under supercritical state. The extracted Ganoderma lucidum spore oil and supercritical CO2 enter the separator from the extraction kettle for separation; 2-3 separators can be set up to separate the product from other impurities (if there are other impurities, such as water, etc.).

[0012] The extracted Ganoderma lucidum spore oil is collected from the separator.

[0013] Furthermore, the guide plate is located between the upper end of the air inlet at the bottom of the extraction kettle and the fluid distributor at the bottom of the material basket. After the supercritical CO2 fluid enters from the air inlet at the bottom of the extractor, it passes through the guide plate, and then passes through the fluid distributor under the material basket, and enters the material basket to contact and transfer mass with the material. A certain number and shape of small holes are drilled on the guide plate, and it is connected to the fluid distributor.

[0014] Furthermore, the CO2 gas source, high-pressure pump, extraction kettle and separator are connected in sequence.

[0015] Furthermore, the extraction pressure in the extraction kettle is 45-55 MPa, preferably 48-53 MPa, and the extraction temperature is 50-65°C, preferably 55-60°C.

[0016] Furthermore, the CO2 flow rate in the extraction kettle is 25-45 kg / h, preferably 35-40 kg / h, and the extraction time is 40-80 min, preferably 50-70 min.

[0017] Furthermore, a condenser is provided between the CO2 gas source and the high-pressure pump, and the condenser is connected to the separator; the CO2 separated from the separator enters the condenser for circulation.

[0018] Furthermore, the temperature in the separator is 49-51° C., and the pressure is 4-5 MPa.

[0019] Furthermore, before extraction, CO2 is introduced into the extraction kettle to replace the air therein.

[0020] Furthermore, the ganoderma lucidum spore powder raw material is wall-broken ganoderma lucidum spore powder.

[0021] Furthermore, a valve for collecting Ganoderma lucidum spore oil is provided at the bottom of the separator.

[0022] Compared with the prior art, the present invention has the following advantages:

[0023] (1) The present invention allows the supercritical CO2 fluid entering the extraction kettle to pass through the fluid distributor at a uniform speed and smoothly under the action of the guide plate, enter the material basket and contact with the material, thereby improving the mass transfer effect and eliminating the raw material granulation pretreatment step;

[0024] (2) The present invention establishes the optimal combination of extraction pressure, extraction temperature and CO2 flow rate, so that the CO2 circulation amount per unit mass of Ganoderma lucidum spore oil extracted is minimized and the extraction time is minimized;

[0025] (3) Under the optimized conditions of the present invention, the CO2 circulation amount and extraction time per unit mass of Ganoderma lucidum spore oil are lower than those in the prior art, which significantly improves the efficiency of extracting Ganoderma lucidum spore oil and reduces the production cost of Ganoderma lucidum spore oil;

[0026] (4) The method of the present invention is simple, green and easy to scale up industrially. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 This is a schematic diagram of the process flow of extracting Ganoderma lucidum spore oil with supercritical CO2 in the present invention;

[0028] Figure 2 The combination of the extraction kettle, fluid distributor and material basket of comparative example (a) and the combination of the guide plate, extraction kettle, fluid distributor and material basket of embodiment (b);

[0029] Figure 3 Digital photos of ungranulated (3A) and granulated (3B) Ganoderma lucidum spore powder raw materials;

[0030] Figure 4 This is a digital photo of the Ganoderma lucidum spore oil extracted by the present invention. DETAILED DESCRIPTION

[0031] The present invention is described in detail below in conjunction with the accompanying drawings and specific embodiments. This embodiment is implemented based on the technical solution of the present invention, and provides a detailed implementation method and specific operation process, but the protection scope of the present invention is not limited to the following embodiments.

[0032] A method for extracting ganoderma spore oil quickly and with high yield by supercritical CO2 without granulation, specifically comprising the following steps:

[0033] (1) After a certain amount of Ganoderma lucidum spore powder raw material is loaded into a stainless steel material basket, it is carefully placed in an extraction kettle, and the extraction kettle lid is covered and tightened. CO2 is introduced into the extraction kettle from a CO2 gas source to replace the air inside the extraction kettle. The CO2 entering the extraction kettle first passes through a guide plate, and then passes through a fluid distributor and enters the material basket to contact and transfer mass with the Ganoderma lucidum spore powder.

[0034] (2) Setting the extraction temperature and extraction pressure, turning on the CO2 high-pressure pump to pump CO2 into the extraction kettle, and when the temperature and pressure of the extraction kettle reach the preset values, opening the regulating valve on the separator, adjusting the CO2 flow rate to the set value, and allowing CO2 to enter the condenser for circulation. The extraction pressure and extraction temperature are set to 45-55MPa and 50-65°C, respectively, and can be further preferably 48-53MPa and 55-60°C, respectively, and the CO2 circulation flow rate is set to 25-45kg / h, and can be further preferably 35-40kg / h;

[0035] (3) The cycle starts, the extraction time is recorded, and when the extraction reaches the set time, the extraction is stopped to end, and then the Ganoderma lucidum spore oil is collected from the bottom of the separator through the valve. After the CO2 in the extraction kettle is recovered, the remaining small amount of CO2 is released to normal pressure, and then the extraction kettle cover is opened to take out the Ganoderma lucidum spore powder. The extraction time is set to 40-80 min, and can be further preferably 50-70 min.

[0036] The ganoderma lucidum spore oil obtained according to the above steps (1) to (3) is weighed, and the yield is calculated according to the weight of the extracted ganoderma lucidum spore oil and the weight of the ganoderma lucidum spore powder raw material. The calculation method is the weight of the extracted ganoderma lucidum spore oil divided by the weight of the ganoderma lucidum spore powder raw material, that is, the extraction yield % = the weight of the extracted ganoderma lucidum spore oil / the weight of the ganoderma lucidum spore powder raw material.

[0037] Example 1

[0038] A method for extracting ganoderma lucidum spore oil quickly and with high yield by supercritical CO2 without granulation, according to Figure 1 As shown in the process flow, weigh 2000 grams of broken wall Ganoderma lucidum spore powder, the appearance of the raw material is as follows Figure 3 As shown in A, pour it into the material basket, then put it into the extraction kettle, cover the kettle cover and tighten it. Put a certain amount of CO2 into the extraction kettle from the CO2 gas source, exhaust the air therein, and after the temperature of the extraction equipment reaches the set value, turn on the high-pressure CO2 pump, pump CO2 into the extraction kettle to a pressure of 48MPa, adjust the separator pressure to 4.5MPa, and control the temperature of the extraction kettle and the separator temperature to 50℃ and 50℃ respectively. Stop after running for 50min at a CO2 flow rate of 30kg / h. Collect the product from the bottom of the separator through a valve to obtain 540 grams of Ganoderma lucidum spore oil, with an extraction yield of 27%. Recover the CO2 in the extraction kettle, release the remaining small amount of CO2 to normal pressure, open the extraction kettle cover, and take out the residual Ganoderma lucidum spore powder.

[0039] Example 2

[0040] A method for extracting ganoderma lucidum spore oil quickly and with high yield by supercritical CO2 without granulation, according to Figure 1 As shown in the process flow, weigh 2000 grams of Ganoderma lucidum spore powder, the appearance of the raw material is as follows Figure 3As shown in A, pour it into the material basket, then put it into the extraction kettle, cover the kettle cover and tighten it. Put a certain amount of CO2 into the extraction kettle from the CO2 gas source, exhaust the air therein, and after the temperature of the extraction equipment reaches the set value, turn on the high-pressure CO2 pump, pump CO2 into the extraction kettle to a pressure of 48MPa, adjust the separator pressure to 4.5MPa, and control the temperature of the extraction kettle and the separator temperature to 50℃ and 50℃ respectively. Stop after running for 70min at a CO2 flow rate of 35kg / h. Collect the product from the bottom of the separator through a valve to obtain 580 grams of Ganoderma lucidum spore oil, with an extraction yield of 29%. Recover the CO2 in the extraction kettle, release the remaining small amount of CO2 to normal pressure, open the extraction kettle cover, and take out the residual Ganoderma lucidum spore powder.

[0041] Example 3

[0042] A method for extracting ganoderma lucidum spore oil quickly and with high yield by supercritical CO2 without granulation, according to Figure 1 As shown in the process flow, weigh 2000 grams of Ganoderma lucidum spore powder, the appearance of the raw material is as follows Figure 3 As shown in A, pour it into the material basket, then put it into the extraction kettle, cover the kettle cover and tighten it. Put a certain amount of CO2 into the extraction kettle from the CO2 gas source, exhaust the air therein, and after the temperature of the extraction equipment reaches the set value, turn on the high-pressure CO2 pump, pump CO2 into the extraction kettle until the pressure is 53MPa, the separator pressure is adjusted to 4.5MPa, the temperature of the extraction kettle and the separator temperature are controlled to 55℃ and 50℃ respectively, and shut down after running for 60min at a CO2 flow rate of 40kg / h. Collect the product from the bottom of the separator through a valve to obtain 600 grams of Ganoderma lucidum spore oil, and the extraction yield is 30%. Recover the CO2 in the extraction kettle, release the remaining small amount of CO2 to normal pressure, open the extraction kettle cover, and take out the residual Ganoderma lucidum spore powder.

[0043] Example 4

[0044] A method for extracting ganoderma lucidum spore oil quickly and with high yield by supercritical CO2 without granulation, according to Figure 1 As shown in the process flow, weigh 2000 grams of Ganoderma lucidum spore powder, the appearance of the raw material is as follows Figure 3As shown in A, pour it into the material basket, then put it into the extraction kettle, cover the kettle cover and tighten it. Put a certain amount of CO2 into the extraction kettle from the CO2 gas source, exhaust the air therein, and after the temperature in the extraction equipment reaches the set value, turn on the high-pressure CO2 pump, pump CO2 into the extraction kettle until the pressure is 58MPa, the separator pressure is adjusted to 4.5MPa, the temperature of the extraction kettle and the separator temperature are controlled to 60℃ and 50℃ respectively, and shut down after running for 80min at a CO2 flow rate of 35kg / h. Collect the product from the bottom of the separator through a valve to obtain 600 grams of Ganoderma lucidum spore oil, and the extraction yield is 30%. Recover part of the CO2 in the extraction kettle, release the remaining small amount of CO2 to normal pressure, and take out the residual Ganoderma lucidum spore powder.

[0045] Comparative Example 1

[0046] The ungranulated Ganoderma lucidum spore powder was used as raw material, and the extraction was carried out under the same extraction process conditions as in Example 3. The difference is that in the extraction kettle, there is no guide plate for supercritical CO2 to pass through, only Figure 2 In the assembly composed of the extraction kettle, the material basket and the fluid distributor shown in A, supercritical CO2 enters the material basket directly through the fluid distributor from the air inlet at the bottom of the extractor to contact and extract the material in the material basket. After the extraction, only 362 grams of ganoderma lucidum spore oil was obtained, which was 238 grams less than that of the ganoderma lucidum spore oil extracted in Example 3, and the extraction yield was reduced to 18.1%. By comparing the results of Comparative Example 1 and Example 3, it is shown that the guide plate designed and constructed in the extractor of the present invention has a great influence on the extraction efficiency.

[0047] Comparative Example 2

[0048] Except that the extraction temperature was 35° C., all other conditions were the same as those in Example 3. After the extraction, 485 g of Ganoderma lucidum spore oil was obtained, and the extraction yield of Ganoderma lucidum spore oil was 24.25%. This indicates that there is an optimal combination of pressure and temperature.

[0049] Comparative Example 3

[0050] Except that the CO2 flow rate was 60 kg / h, all other conditions were the same as those in Example 3. After the extraction, 518 g of Ganoderma lucidum spore oil was obtained, and the extraction yield of Ganoderma lucidum spore oil was 25.9%. This shows that the larger the flow rate, the better, and the flow rate also has an optimal value. There is an optimal combination of pressure, temperature, and flow rate.

[0051] The above is only a preferred embodiment of the present invention, and does not limit the present invention in other forms. Any technician familiar with the profession may use the above disclosed technical content to change or modify it into an equivalent embodiment with equivalent changes. However, any simple modification, equivalent change and modification made to the above embodiment according to the technical essence of the present invention, especially the change of the structure of the guide plate, which does not deviate from the technical solution of the present invention, still belongs to the protection scope of the technical solution of the present invention.

Claims

1. A method for extracting Ganoderma lucidum spore oil by supercritical extraction without granulation, characterized in that: The method comprises the following steps: After the ganoderma lucidum spore powder raw material is loaded into the material basket, the material basket is then placed in the extraction kettle, and the extraction kettle is sealed; the extraction kettle is provided with a guide plate for changing the flow state of the supercritical CO2 fluid before entering the fluid distributor, so that the supercritical CO2 fluid passes through the fluid distributor at a uniform speed and stably to contact and transfer mass with the material in the material basket; The CO2 in the CO2 gas source is pumped into the extraction kettle through a high-pressure pump, and extraction is performed under a supercritical state, and the extracted Ganoderma lucidum spore oil and supercritical CO2 are separated by entering a separator from the extraction kettle; collecting the extracted Ganoderma lucidum spore oil from the separator; The guide plate is located between the upper end of the air inlet at the bottom of the extraction kettle and the fluid distributor at the bottom of the material basket. After the supercritical CO2 fluid enters from the air inlet at the bottom of the extractor, it passes through the guide plate and then passes through the fluid distributor under the material basket to enter the material basket for contact and mass transfer with the material. The CO2 gas source, high-pressure pump, extraction kettle and separator are connected in sequence; the extraction pressure in the extraction kettle is 45-55MPa, and the extraction temperature is 50-65°C; The CO2 flow rate in the extraction kettle is 25-45 kg / h, and the extraction time is 40-80 min.

2. The method for supercritical extraction of Ganoderma lucidum spore oil without granulation according to claim 1, characterized in that: The extraction pressure in the extraction kettle is 48-53 MPa, and the extraction temperature is 55-60°C.

3. The method for supercritical extraction of Ganoderma lucidum spore oil without granulation according to claim 1, characterized in that: The CO2 flow rate in the extraction kettle is 35-40 kg / h, and the extraction time is 50-70 min.

4. The method for supercritical extraction of Ganoderma lucidum spore oil without granulation according to claim 1, characterized in that: A condenser is provided between the CO2 gas source and the high-pressure pump, and the condenser is connected to the separator; the CO2 separated from the separator enters the condenser for circulation.

5. The method for supercritical extraction of Ganoderma lucidum spore oil without granulation according to claim 1, characterized in that: The temperature in the separator is 49-51°C, and the pressure is 4-5MPa.

6. The method for supercritical extraction of Ganoderma lucidum spore oil without granulation according to claim 1, characterized in that: Before extraction, CO2 is introduced into the extraction kettle to replace the air inside.

7. The method for supercritical extraction of Ganoderma lucidum spore oil without granulation according to claim 1, characterized in that: The ganoderma lucidum spore powder raw material is wall-broken ganoderma lucidum spore powder.

8. The method for supercritical extraction of Ganoderma lucidum spore oil without granulation according to claim 1, characterized in that: A valve for collecting ganoderma spore oil is arranged at the bottom of the separator.

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