Patent Application
20250083067
The present application claims priority to the Chinese Patent Application No. 202210649001.3, filed with the China National Intellectual Property Administration (CNIPA) on Jun. 9, 2022, and entitled “METHOD FOR ENHANCED SEPARATION OF ORGANIC MATTERS IN MIXED COMPONENT WITH SUPERCRITICAL FLUID COMBINATION MEDIUM”, which is incorporated herein by reference in its entirety.
The present disclosure relates to the technical field of supercritical fluids, in particular to a method for enhanced separation of organic matters in a mixed component with a supercritical fluid combination medium.
Supercritical fluid separation of a mixed component refers to contacting a supercritical fluid with a mixed component to be separated in a supercritical state. By introducing a cosolvent suitable for component separation requirements, components with different polar characteristics, boiling points, and molecular weights can be selectively separated (referring to: Tiancheng Mu, Buxing Han. Progress in Cosolvent Effect of Supercritical Fluids and Mixed Fluids [J]. Progress in Chemistry, 2006, 18 (1): 5).
Due to its liquid-like density and gas-like low viscosity, supercritical fluids have excellent solubility for macromolecular organic matters. Supercritical CO2 has lower critical temperature and critical pressure, and is easier to form a combination medium with other reagents for separating natural mixed components. When water and/or other types of solvents as a cosolvent are introduced into the supercritical CO2, polarity of the combination medium can be changed only by adjusting relevant parameters of the supercritical fluid. In this way, a dissolution effect of the combination medium can be adjusted on different natural mixed components. At present, there are mainly two existing methods for the separation of a mixed component with the supercritical fluid combination medium. One is to immerse the mixed component into a cosolvent of the supercritical fluid combination medium, and separate the mixed component under fixed environmental state parameters. Since the mixed component is not in direct contact with the supercritical fluid, a separation effect of the supercritical fluid is not fully exerted. As a result, a separation efficiency of the method and a yield of obtained separated components need to be improved. The other is to set flow rates of the supercritical carbon dioxide and the cosolvent, respectively, such that the supercritical fluid combination medium passes through a separation device filled with the mixed component at a certain flow rate. In this method, a supercritical fluid circulation process has high energy consumption, consumption of the cosolvent, and cost.
In view of this, an objective of the present disclosure is to provide a method for enhanced separation of organic matters in a mixed component with a supercritical fluid combination medium. In the present disclosure, the method can effectively improve a separation efficiency and a yield of obtained separated components, and has low consumption of a cosolvent.
To achieve the above objective, the present disclosure provides the following technical solutions:
The present disclosure provides a method for enhanced separation of organic matters in a mixed component with a supercritical fluid combination medium, where the supercritical fluid combination medium includes a supercritical fluid and a cosolvent; and the method includes the following steps:
Preferably, the supercritical fluid is one or more selected from the group consisting of supercritical CO2, supercritical water, supercritical ethanol, supercritical methanol, supercritical ammonia, and a supercritical alkane.
Preferably, the cosolvent is water and/or an organic alcohol.
Preferably, the supercritical fluid and the cosolvent are at a molar ratio of 1:1 to 1:10.
Preferably, the mixed component and the cosolvent are at a mass-to-volume ratio of 1 g:(1-15) mL.
Preferably, the supercritical fluid separation is conducted at 31.26° C. to 200° C. and a pressure of 7.38 MPa to 65 MPa for 10 min to 180 min.
Preferably, the separation temperature is periodically changed 1 to 10 times.
Preferably, a process of changing the separation temperature periodically includes:
periodically increasing or decreasing the separation temperature by 5° C. to 100° C.
Preferably, the mixed component is a natural mixed component and/or an artificially synthetic mixed component.
Preferably, the natural mixed component is one or more selected from the group consisting of a plant tissue, an animal tissue, and a rock formation containing organic matters.
Preferably, the plant tissue is one or more selected from the group consisting of a Cannabis sativa stalk fiber, an eucalyptus fiber, a bamboo fiber, Balsa wood, and Paulownia; and
the animal tissue is one or more selected from the group consisting of a natural dairy product, an animal fat, and an animal carapace.
Preferably, the artificially synthetic mixed component is one or more selected from the group consisting of waste plastics, waste rubber, and ink-containing waste paper.
Preferably, when lignin is separated from a plant fiber, the separation temperature fluctuates 1 to 5 times at an interval of 100° C. to 200° C., and a heat preservation time in a constant-temperature stage is 5 min to 30 min.
Preferably, when astaxanthin is separated from the animal tissue, the separation temperature fluctuates 1 to 5 times at an interval of 31.26° C. to 70° C. under a pressure of 30 MPa to 65 MPa, and a heat preservation time in a constant-temperature stage is 1 min to 10 min.
Preferably, when cholesterol is separated from the natural dairy product, the separation temperature fluctuates 1 to 5 times at an interval of 31.26° C. to 70° C. under a pressure of 7 MPa to 15 MPa, and a heat preservation time in a constant-temperature stage is 1 min to 10 min.
Preferably, when a fatty acid is separated from the animal fat, the separation temperature fluctuates 1 to 5 times at an interval of 31.26° C. to 50° C. under a pressure of 8 MPa to 20 MPa, and a heat preservation time in a constant-temperature stage is 60 min to 200 min.
The present disclosure provides a method for enhanced separation of organic matters in a mixed component with a supercritical fluid combination medium, where the supercritical fluid combination medium includes a supercritical fluid and a cosolvent; and the method includes the following steps: placing a mixed component to be separated and the cosolvent in a reaction vessel, suspending the mixed component to be separated above a liquid level line of the cosolvent, and introducing the supercritical fluid into the reaction vessel to conduct supercritical fluid separation; where during the supercritical fluid separation, a separation temperature is changed periodically within a supercritical temperature range of the supercritical fluid combination medium. In the present disclosure, a traditional treatment method of immersing a mixed component in a cosolvent is changed, the mixed component and the cosolvent are placed in a reaction vessel, and the mixed component is not in contact with the cosolvent, that is, a liquid phase non-contact method is adopted. On one hand, a dosage of the cosolvent can be reduced. On the other hand, during the supercritical fluid separation, the mixed component can fully contact with the supercritical fluid, such that an effect of the supercritical fluid can be fully exerted, and a separation efficiency and a yield of obtained separated components can be improved. The separation temperature of the supercritical fluid is periodically changed, and the supercritical fluid combination medium has characteristic parameters that change with temperatures, so as to obtain a higher separation yield with low energy consumption. In this way, a separation time is shortened. Specifically, when the temperature changes periodically, a supercritical phase-liquid phase boundary line of the supercritical fluid combination medium is not stable in the space. The densities of the supercritical phase and the cosolvent liquid phase fluctuate dynamically within a certain range, resulting in a strong material exchange between the supercritical phase and the liquid phase. As a result, the migration of obtained separated components by the supercritical fluid combination medium is accelerated, thereby enhancing a separation effect of the supercritical fluid combination medium.
The present disclosure provides a method for enhanced separation of organic matters in a mixed component based on a supercritical fluid combination medium, where the supercritical fluid combination medium includes a supercritical fluid and a cosolvent; and the method includes the following steps:
In the present disclosure, the mixed component is a mixed component containing organic matters and suitable for component separation using a supercritical fluid. The mixed component is preferably a natural mixed component and/or an artificially synthetic mixed component.
In the present disclosure, the natural mixed component is preferably one or more selected from the group consisting of a plant tissue, an animal tissue, and a rock formation containing organic matters.
In the present disclosure, the plant tissue is preferably one or more selected from the group consisting of Cannabis sativa stalk fiber, an eucalyptus fiber, a bamboo fiber, Balsa wood, and Paulownia. When the natural mixed component is a plant fiber, preferably lignin and/or hemicellulose in the plant fiber is separated and extracted.
In the present disclosure, the animal tissue is preferably one or more selected from the group consisting of a natural dairy product, an animal fat, and an animal carapace. The natural dairy product is preferably one or more selected from the group consisting of milk, a whole milk powder, and a pure milk powder. When the natural mixed component is the natural dairy product, preferably cholesterol in the natural dairy product is separated and extracted. There is no special requirement on a type of the animal fat. When the natural mixed component is the animal fat, preferably a fatty acid in the animal fat is separated and extracted.
In the present disclosure, the artificially synthetic mixed component is preferably one or more selected from the group consisting of waste plastics, waste rubber, and ink-containing waste paper. The waste plastics are preferably plastic lunch boxes and/or express bags.
In the present disclosure, when the artificially synthetic mixed component is the waste plastics, preferably a grease in the waste plastics is separated and extracted. When the artificially synthetic mixed component is the waste rubber, preferably an engine oil in the waste rubber is separated and extracted. When the artificially synthetic mixed component is the ink-containing waste paper, preferably ink in the waste paper is separated and extracted.
In the present disclosure, a mixed component to be separated and a cosolvent are placed in a reaction vessel, and the mixed component to be separated and the cosolvent are not in contact with each other to conduct supercritical fluid separation. The mixed component has a particle size of preferably 20 mesh to 200 mesh, more preferably 50 to 150 mesh. When the mixed component has a particle size of greater than 20 mesh, the mixed component is preferably pulverized. There is no special requirement on a pulverization method, and pulverization methods well known to those skilled in the art can be used.
In the present disclosure, the reaction vessel is preferably provided with a screen inside, such that the mixed component is suspended above the liquid level line of the cosolvent, and the mixed component does not contact with the cosolvent.
In the present disclosure, the supercritical fluid is preferably one or more selected from the group consisting of supercritical CO2, supercritical water, supercritical ethanol, supercritical methanol, supercritical ammonia, and a supercritical alkane.
In the present disclosure, the cosolvent is preferably water and/or an organic alcohol, and the organic alcohol is preferably methanol and/or ethanol. As a specific example, the cosolvent includes water and ethanol.
In the present disclosure, in the supercritical fluid combination medium, the supercritical fluid and the cosolvent are at a molar ratio of 1:1 to 1:10, more preferably 1:1 to 1:5.
In the present disclosure, the supercritical fluid separation is conducted at preferably 31.26° C. to 200° C., more preferably 31.26° C. to 50° C. and a pressure of preferably 7.38 MPa to 35 MPa, more preferably 10 MPa to 30 MPa for preferably 10 min to 180 min, more preferably 30 min to 150 min.
In the present disclosure, a process of periodically changing the separation temperature includes: periodically increasing or decreasing the separation temperature. An increased or decreased separation temperature is still within a supercritical temperature range of the supercritical fluid combination medium. The separation temperature is preferably increased or decreased by 5° C. to 100° C., more preferably 20° C. to 60° C., and even more preferably 30° C. to 50° C. A cycle of periodically changing the separation temperature includes constant-temperature stage and a variable-temperature stage, and a single constant-temperature stage lasts for preferably 5 min to 30 min, more preferably 10 min to 20 min.
In the present disclosure, when periodically changing the separation temperature refers to periodically increasing the separation temperature, the variable-temperature stage includes preferably heating and cooling to a constant temperature. The heating is conducted at preferably 5° C./min to 20° C./min, more preferably 10° C./min to 15° C./min; and the cooling to a constant temperature is conducted at preferably 10° C./min to 30° C./min, more preferably 15° C./min to 25° C./min.
In the present disclosure, when periodically changing the separation temperature refers to periodically reducing the separation temperature, the variable-temperature stage includes preferably cooling and heating to a constant temperature. The cooling is conducted at preferably 10° C./min to 30° C./min, more preferably 15° C./min to 25° C./min; and the heating to a constant temperature is conducted at preferably 5° C./min to 20° C./min, more preferably 10° C./min to 15° C./min.
In the present disclosure, a single variable-temperature stage lasts for preferably 10 min to 40 min, more preferably 20 min to 30 min.
In the present disclosure, the separation temperature is preferably periodically changed 1 to 10 times, more preferably 1 to 4 times.
In the present disclosure, according to different objects to be separated, the temperature setting needs to match the characteristics of a separated substance. Specifically, when lignin is separated from a plant fiber, the separation temperature fluctuates preferably 1 to 5 times at an interval of 100° C. to 200° C., and a heat preservation time in a constant-temperature stage is preferably 5 min to 30 min.
When astaxanthin is separated from the animal tissue such as shrimp shells, the separation temperature fluctuates preferably 1 to 5 times at an interval of 31.26° C. to 70° C. under a pressure of 30 MPa to 65 MPa, and a heat preservation time in a constant-temperature stage is preferably 1 min to 10 min.
When cholesterol is separated from the natural dairy product, the separation temperature fluctuates preferably 1 to 5 times at an interval of 31.26° C. to 70° C. under a pressure of 7 MPa to 15 MPa, and a heat preservation time in a constant-temperature stage is preferably 1 min to 10 min.
When a fatty acid is separated from the animal fat, the separation temperature fluctuates preferably 1 to 5 times at an interval of 31.26° C. to 50° C. under a pressure of 8 MPa to 20 MPa, and a heat preservation time in a constant-temperature stage is preferably 60 min to 200 min.
In the present disclosure,
In a coordinate system formed by temperature, pressure, and density, a density gradient behavior of various supercritical fluid combination media presents a strong change trend. When the temperature changes periodically, a supercritical phase-liquid phase boundary line of the supercritical fluid combination medium is not stable in the space. The densities of the supercritical phase and the liquid phase fluctuate dynamically within a certain range, resulting in a strong material exchange between the supercritical phase and the liquid phase. As a result, the migration of obtained separated components by the supercritical fluid combination medium is accelerated, thereby enhancing a separation effect of the supercritical fluid combination medium.
The method for enhanced separation of organic matters in a mixed component with a supercritical fluid combination medium provided by the present disclosure are described in detail below with reference to the examples, but these examples may not be understood as a limitation to the protection scope of the present disclosure.
12.5 g of Cannabis sativa stalk fiber was taken (with a hemicellulose content of 14.8%). A liquid-to-solid ratio was set at 10:1 (V:m), and 125 mL of deionized water was injected into a separation device. A sample to be treated was suspended above a liquid level line, the separation device was pressed tightly, and CO2 was injected. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 6 MPa. When the temperature rose to 458.85 K, a separation process of hemicellulose in the Cannabis sativa stalk fiber was controlled according to a temperature control procedure shown in
12.5 g of Cannabis sativa stalk fiber was taken (with a hemicellulose content of 14.8%). A liquid-to-solid ratio was set at 10:1 (V:m), and 125 mL of deionized water was injected into a separation device. A sample to be treated was suspended above a liquid level line, the separation device was pressed tightly, and CO2 was injected. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 6 MPa. When the temperature rose to 458.85 K, a separation process of hemicellulose in the Cannabis sativa stalk fiber was controlled according to a temperature control procedure shown in
12.5 g of eucalyptus fiber was taken (with a hemicellulose content of 16%). A liquid-to-solid ratio was set at 10:1 (V:m), and 125 mL of deionized water was injected into a separation device. A sample to be treated was suspended above a liquid level line, the separation device was pressed tightly, and CO2 was injected. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 6 MPa. When the temperature rose to 458.85 K, a separation process of hemicellulose in the eucalyptus fiber was controlled according to a temperature control procedure shown in
12.5 g of eucalyptus fiber was taken (with a hemicellulose content of 16%). A liquid-to-solid ratio was set at 10:1 (V:m), and 125 mL of deionized water was injected into a separation device. A sample to be treated was suspended above a liquid level line, the separation device was pressed tightly, and CO2 was injected. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 6 MPa. When the temperature rose to 458.85 K, a separation process of hemicellulose in the eucalyptus fiber was controlled according to a temperature control procedure shown in
12.5 g of Cannabis sativa stalk fiber was taken (with a lignin content of 22%). A liquid-to-solid ratio was set at 10:1 (V:m), 125 mL of an EtOH—H2O solution with a molar ratio of 1:1 was added to a separation device, and CO2 was injected. A sample to be treated was suspended above a liquid level line, and the separation device was pressed tightly. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 6 MPa. When the temperature rose to 458.85 K, a separation process of lignin in the Cannabis sativa stalk fiber was controlled according to a temperature control procedure shown in
12.5 g of Cannabis sativa stalk fiber was taken (with a lignin content of 22%). A liquid-to-solid ratio was set at 10:1 (V:m), 125 mL of an EtOH—H2O solution with a molar ratio of 1:1 was added to a separation device, and CO2 was injected. A sample to be treated was suspended above a liquid level line, and the separation device was pressed tightly. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 6 MPa. When the temperature rose to 458.85 K, a separation process of lignin in the Cannabis sativa stalk fiber was controlled according to a temperature control procedure shown in
12.5 g of eucalyptus fiber was taken (with a lignin content of 33.7%). A liquid-to-solid ratio was set at 10:1 (V:m), 125 mL of an EtOH—H2O solution with a molar ratio of 1:1 was added to a separation device, and CO2 was injected. A sample to be treated was suspended above a liquid level line, and the separation device was pressed tightly. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 6 MPa. When the temperature rose to 458.85 K, a separation process of lignin in the eucalyptus fiber was controlled according to a temperature control procedure shown in
12.5 g of eucalyptus fiber was taken (with a lignin content of 33.7%). A liquid-to-solid ratio was set at 10:1 (V:m), 125 mL of an EtOH—H2O solution with a molar ratio of 1:1 was added to a separation device, and CO2 was injected. A sample to be treated was suspended above a liquid level line, and the separation device was pressed tightly. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 6 MPa. When the temperature rose to 458.85 K, a separation process of lignin in the eucalyptus fiber was controlled according to a temperature control procedure shown in
80 g of whole milk powder was taken (with a cholesterol content of 6.1547 mg/100 g). A liquid-to-solid ratio was set at 1:1 (V:m), and 80 mL of ethanol was injected into a separation device. A sample to be treated was suspended above a liquid level line, the separation device was pressed tightly, and CO2 was injected. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 10 MPa. When the temperature rose to 331.15 K, a separation process of cholesterol in the whole milk powder was controlled according to a temperature control procedure shown in
80 g of whole milk powder was taken (with a cholesterol content of 6.1547 mg/100 g). A liquid-to-solid ratio was set at 1:1 (V:m), and 80 mL of ethanol was injected into a separation device. A sample to be treated was suspended above a liquid level line, the separation device was pressed tightly, and CO2 was injected. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 10 MPa. When the temperature rose to 331.15 K, a separation process of cholesterol in the whole milk powder was controlled according to a temperature control procedure shown in
15 g of recycled plastic lunch boxes were taken (with a greasy dirt mass of 3 g). A liquid-to-solid ratio was set at 10:1, and 250 mL of ethanol was injected into a separation device. A sample to be treated was suspended above a liquid level line, the separation device was pressed tightly, and CO2 was injected. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 6 MPa. When the temperature rose to 350.15 K, a separation process of greasy dirt in the recycled plastic lunch boxes was controlled according to a temperature control procedure shown in
15 g of recycled plastic lunch boxes were taken (with a greasy dirt mass of 3 g). A liquid-to-solid ratio was set at 10:1, and 250 mL of ethanol was injected into a separation device. A sample to be treated was suspended above a liquid level line, the separation device was pressed tightly, and CO2 was injected. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 6 MPa. When the temperature rose to 350.15 K, a separation process of greasy dirt in the recycled plastic lunch boxes was controlled according to a temperature control procedure shown in
12.5 g of Cannabis sativa stalk fiber was taken (with a hemicellulose content of 14.8%). A liquid-to-solid ratio was set at 10:1 (V:m), and 125 mL of deionized water was injected into a separation device. A sample to be treated was immersed in the deionized water, the separation device was pressed tightly, and CO2 was injected. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 6 MPa. When the temperature rose to 458.85 K, constant temperature and pressure were kept. After 100 min, an extraction rate of a product xylan was 1.35 g/100 g.
12.5 g of Cannabis sativa stalk fiber was taken (with a hemicellulose content of 14.8%). A liquid-to-solid ratio was set at 10:1 (V:m), and 125 mL of deionized water was injected into a separation device. A sample to be treated was suspended above a liquid level line, the separation device was pressed tightly, and CO2 was injected. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 6 MPa. When the temperature rose to 458.85 K, constant temperature and pressure were kept. After 100 min, an extraction rate of a hemicellulose degradation product xylan could reach 0.96 g/100 g of raw materials.
12.5 g of eucalyptus fiber was taken (with a hemicellulose content of 16%). A liquid-to-solid ratio was set at 10:1 (V:m), and 125 mL of deionized water was injected into a separation device. A sample to be treated was immersed in the deionized water, the separation device was pressed tightly, and CO2 was injected. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 6 MPa. When the temperature rose to 458.85 K, constant temperature and pressure were kept. After 100 min, an extraction rate of a product xylan was 3.69 g/100 g.
12.5 g of eucalyptus fiber was taken (with a hemicellulose content of 16%). A liquid-to-solid ratio was set at 10:1 (V:m), and 125 mL of deionized water was injected into a separation device. A sample to be treated was suspended above a liquid level line, the separation device was pressed tightly, and CO2 was injected. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 6 MPa. When the temperature rose to 458.85 K, constant temperature and pressure were kept. After 100 min, a yield of a hemicellulose degradation product xylan could reach 1.54 g/100 g of raw materials.
12.5 g of Cannabis sativa stalk fiber was taken (with a lignin content of 22%). A liquid-to-solid ratio was set at 10:1 (V:m), and 125 mL of an EtOH—H2O solution with a molar ratio of 1:1 was added to a separation device. A sample to be treated was immersed in the EtOH—H2O solution, the separation device was pressed tightly, and CO2 was injected. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 6 MPa. When the temperature rose to 458.85 K, constant temperature and pressure were kept. After 100 min, a yield of a product Klason lignin reached 29.3%.
12.5 g of Cannabis sativa stalk fiber was taken (with a lignin content of 22%). A liquid-to-solid ratio was set at 10:1 (V:m), 125 mL of an EtOH—H2O solution with a molar ratio of 1:1 was added to a separation device. A sample to be treated was suspended above a liquid level line, the separation device was pressed tightly, and CO2 was injected. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 6 MPa. When the temperature rose to 458.85 K, constant temperature and pressure were kept. After 100 min, a yield of a product Klason lignin reached 26.4%.
12.5 g of eucalyptus fiber was taken (with a lignin content of 33.7%). A liquid-to-solid ratio was set at 10:1 (V:m), and 125 mL of an EtOH—H2O solution with a molar ratio of 1:1 was added to a separation device. A sample to be treated was immersed in the EtOH—H2O solution, the separation device was pressed tightly, and CO2 was injected. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 6 MPa. When the temperature rose to 458.85 K, constant temperature and pressure were kept. After 100 min, a yield of a product Klason lignin reached 45.2%.
12.5 g of eucalyptus fiber was taken (with a lignin content of 33.7%). A liquid-to-solid ratio was set at 10:1 (V:m), 125 mL of an EtOH—H2O solution with a molar ratio of 1:1 was added to a separation device. A sample to be treated was suspended above a liquid level line, the separation device was pressed tightly, and CO2 was injected. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 6 MPa. When the temperature rose to 458.85 K, constant temperature and pressure were kept. After 100 min, a yield of a product Klason lignin reached 41.9%.
80 g of whole milk powder was taken (with a cholesterol content of 6.1547 mg/100 g). A liquid-to-solid ratio was set at 1:1 (V:m), and 80 mL of ethanol was injected into a separation device. A sample to be treated was immersed into the ethanol, the separation device was pressed tightly, and CO2 was injected. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 10 MPa. When the temperature rose to 331.15 K, constant temperature and pressure were kept. A separation rate of a product cholesterol could reach 10.2%.
80 g of whole milk powder was taken (with a cholesterol content of 6.1547 mg/100 g). A liquid-to-solid ratio was set at 1:1 (V:m), and 80 mL of ethanol was injected into a separation device. A sample to be treated suspended above a liquid level line, the separation device was pressed tightly, and CO2 was injected. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 10 MPa. When the temperature rose to 331.15 K, constant temperature and pressure were kept. After 100 min, a separation rate of a product cholesterol could reach 5.7%.
15 g of recycled plastic lunch boxes were taken (with a greasy dirt mass of 3 g). A liquid-to-solid ratio was set at 10:1, and 250 mL of ethanol was injected into a separation device. A sample to be treated was immersed into the ethanol, the separation device was pressed tightly, and CO2 was injected. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 6 MPa. When the temperature rose to 350.15 K, constant temperature and pressure were kept. A separation rate of the greasy dirt could reach 36.9%.
15 g of recycled plastic lunch boxes were taken (with a greasy dirt mass of 3 g). A liquid-to-solid ratio was set at 10:1, and 250 mL of ethanol was injected into a separation device. A sample to be treated suspended above a liquid level line, the separation device was pressed tightly, and CO2 was injected. An initial temperature and an initial pressure of an obtained system were adjusted to 303.15 K and 6 MPa. When the temperature rose to 350.15 K, constant temperature and pressure were kept. After 100 min, a separation rate of the greasy dirt could reach 79.6%.
The data of the foregoing examples were compared, as shown in Table 1.
Cannabis sativa
Cannabis sativa
It was seen from Table 1 that the method of non-contact with liquid phase and periodically changing the separation temperature provided by the present disclosure could effectively increase a yield of organic matters.
The above are merely preferred implementations of the present disclosure. It should be noted that several improvements and modifications may further be made by a person of ordinary skill in the art without departing from the principle of the present disclosure, and such improvements and modifications should also be deemed as falling within the protection scope of the present disclosure.
| Number | Date | Country | Kind |
|---|---|---|---|
| 202210649001.3 | Jun 2022 | CN | national |
| Filing Document | Filing Date | Country | Kind |
|---|---|---|---|
| PCT/CN2022/119335 | 9/16/2022 | WO |
