Agilawood extract pneumatic control type supercritical extraction equipment and process

Abstract

The present invention discloses an agilawood extract pneumatic control type supercritical extraction apparatus and process, and relates to the technical field of supercritical extraction, the agilawood extract pneumatic control type supercritical extraction apparatus comprises: an ultrasonic extraction tank for accommodating an extracted agilawood extract, and the agilawood extract forms a material bed layer in the ultrasonic extraction tank; one end of the dynamic adjustable distributor is connected into the gas tank, the other end of the dynamic adjustable distributor is inserted into the ultrasonic extraction tank from the bottom of the ultrasonic extraction tank, and carbon dioxide in the gas tank is uniformly or directionally distributed on the cross section of the agilawood extract bed layer after passing through the gas distributor; by switching the two modes, the distribution mode of the fluid can be dynamically adjusted along with the extraction process so as to adapt to mass transfer dynamics requirements of different extraction stages, so that the extraction time is further shortened, the yield of components difficult to extract is improved, targeted adjustment is realized, and the process efficiency is improved. And the difficult-to-extract and locally-blocked area is impacted by directional jet flow and concentrated energy, so that the extraction effect is improved.

Description

Technical Field

[0001] This invention relates to the field of supercritical extraction technology, and in particular to a gas-controlled supercritical extraction device and process for agarwood extract. Background Technology

[0002] Agarwood, the resinous wood of the Aquilaria sinensis plant (family Thymelaeaceae), possesses properties that promote qi circulation and relieve pain, warm the stomach and stop vomiting, and regulate qi and relieve asthma. It is commonly used for symptoms such as chest and abdominal distension and pain, stomach cold with vomiting and hiccups, and kidney deficiency with shortness of breath. Traditional agarwood preparations are mostly in the form of pills or powders, which have drawbacks such as long disintegration time and low bioavailability. Droplets, as a novel dosage form, have advantages such as rapid onset of action, high bioavailability, and convenient administration. However, some problems exist in the production process of agarwood droplets currently on the market, such as poor pellet formation, long dissolution time, and unstable content of active ingredients, affecting product quality and efficacy.

[0003] In the preparation of agarwood extract, ethanol is often used as the solvent. To achieve a high extraction rate, liquid CO2 is typically pumped into the extraction vessel at a high flow rate in the initial stages of extraction to quickly build pressure. This high-speed fluid, like a jet, directly impacts the material bed, which may lead to: Bed channeling: The impact force creates one or more channels in a dense bed of material. Subsequent CO2 will preferentially pass through these channels with low resistance, while material in other areas cannot be effectively wetted, resulting in incomplete extraction.

[0004] Uneven distribution: After liquid CO2 enters the huge vessel space from the single inlet pipe at the bottom of the extraction vessel, it is difficult to distribute it evenly across the entire cross-section of the vessel instantly, resulting in excessively high local flow velocities: the area directly above the inlet has the highest flow velocity and the most severe impact.

[0005] For some materials with high oil content or inherent viscosity, the extraction of agarwood extract can increase the amount of ethanol during the extraction process, leading to increased fluid polarity, changes in viscosity, and blockage in some areas. Under normal flow rates, CO2 cannot effectively penetrate its dense structure, resulting in extremely low extraction efficiency. Summary of the Invention

[0006] The purpose of this invention is to provide a gas-controlled supercritical fluid extraction device, process, and apparatus for agarwood extract. This device features two modes that can be switched to dynamically adjust the fluid distribution pattern as the extraction process progresses, adapting to the mass transfer kinetics requirements of different extraction stages. This further shortens the extraction time, increases the yield of difficult-to-extract components, and achieves targeted adjustments, thereby improving process efficiency. Furthermore, it utilizes directional jets to concentrate energy and impact difficult-to-extract or locally blocked areas, enhancing the extraction effect.

[0007] To achieve the above objectives, the present invention provides the following technical solution: a gas-controlled supercritical extraction device for agarwood extract, comprising: An ultrasonic extraction vessel contains agarwood extract to be extracted, and the agarwood extract forms a material bed within the ultrasonic extraction vessel; A dynamic adjustable distributor is connected at one end to the gas tank and inserted into the bottom of the ultrasonic extraction tank at the other end. After passing through the gas distributor, the carbon dioxide in the gas tank is evenly or directionally distributed on the cross-section of the agarwood extract bed. The dynamically adjustable distributor includes a distribution plate that divides the interior of the ultrasonic extraction tank into upper and lower chambers. The distribution plate has a chamber inside, and several main holes on the top of the distribution plate communicate with the chamber. Several directional plates are also installed inside the distribution plate, wherein several exhaust pipes on the top of the directional plates correspond to the number and position of the main holes. A switching component is used to connect the gas tank to a distribution plate or a directional plate. The switching function is achieved by the directional plate moving up and down in the chamber. If none of the directional plates move upward, the carbon dioxide discharged from the gas tank will be discharged from the main hole of the distribution plate and evenly distributed on the agarwood extract bed. When one of the directional plates moves upward, the exhaust pipe is inserted into the main hole, and the carbon dioxide discharged from the gas tank is directionally distributed on the agarwood extract bed.

[0008] As an optional implementation, the ultrasonic extraction vessel is equipped with an ultrasonic generator and an ethanol concentration sensor, and a heating jacket is also fitted over the outside of the ultrasonic extraction vessel.

[0009] As an optional implementation, the top of the distribution plate is provided with a top chamber, wherein the top chamber is connected to the main hole through a side hole, and a one-way device is installed in the main hole below the top chamber.

[0010] As an optional implementation, the one-way device includes a lower ring, an upper ring, a lower seat, an upper seat, and a side rod. The lower ring is fixed to the bottom end of the main hole, the lower seat is fixed to the lower ring, and both the lower seat and the lower ring have through holes. The upper ring is sealed to the main hole, and the guide rod fixed to the bottom end of the upper ring is inserted into the lower seat. The upper ring and the lower seat are also connected by a spring. The inner circumferential surface of the upper ring is connected to the upper seat via a side rod, forming a gas channel between the upper ring and the upper seat. The upper seat is used to seal or open the lower hole.

[0011] As an optional implementation, an ejection mechanism is mounted on the top end of the exhaust pipe. The ejection mechanism includes an ejector rod and a support frame, with the ejector rod fixed to the exhaust pipe via the support frame.

[0012] As an optional implementation, the exhaust pipe moves upward through the lower hole, the push rod first contacts the upper seat and then pushes the upper ring to move upward along the main hole, and is used to seal the side hole. The carbon dioxide in the gas tank is discharged into the ultrasonic extraction tank through the gas channel.

[0013] As an optional implementation, the switching component includes an outer switching tube, an inner switching tube, a locking block, a limiting seat, a hydraulic component, and a sealing plate. The outer switching tube and the inner switching tube are concentrically arranged in the chamber, wherein the inner switching tube is connected to the top chamber and the gas tank. The number of limiting seats is the same as that of the directional plates. The limiting seats are fixed on the outer wall of the switching inner tube. The secondary hole one opened on the limiting seat is connected to the switching inner tube. One end of the directional plate is connected to the locking block. The other end of the locking block passes through the strip groove of the switching outer tube and is locked on the limiting seat. The secondary hole two opened on the locking block is connected to the inner cavity of the directional plate. The exhaust pipe is also connected to the inner cavity. The hydraulic component is fitted onto the switching inner tube and located above the limiting seat, and is connected to the sealing plate.

[0014] As an optional implementation, when the directional plate moves upward for directional distribution, the hydraulic components drive the sealing plate to seal the switching inner tube, and the secondary hole one and secondary hole two are connected.

[0015] As an optional implementation, the orientation plate is driven to move by cylinders inside the chamber, and the number of cylinders is the same as the number of orientation plates.

[0016] An extraction process for agarwood extract includes the following steps: S1: Processing of Agarwood Raw Materials: S11: Raw material selection: Select agarwood blocks of consistent quality; S12: Crushing process: Use a dedicated crusher to crush the material, then pass it through a 20-40 mesh sieve; S13: Moisture control: Adjust the moisture content to 8-12%; S2: Extraction tank filling: S21: Distributor check: Confirm that the adjustable distributor is fully open; S22: Layered filling: Layered compaction filling method is adopted; S23: Filling height: Control the filling height to 70-80% of the effective height of the extraction vessel; S3: Control parameter initialization: S31: The distributor is set to uniform distribution; S4: Extraction: S41: The extraction tank is pressurized to 25-35 MPa and the temperature is increased to 40-50℃. The carbon dioxide flow rate is 20-30 L / h, the ethanol concentration is 70%-80%, and the material-liquid ratio is 1:10-1:15. Combined with ultrasonic-assisted ethanol extraction of non-volatile components, the ultrasonic power is 300W and the time is 30min. The distributor is used in a uniform distribution mode to extract volatile oil. S42: Mode switching: When the extraction rate drops to 60-70% of the peak value, the bed pressure drop tends to stabilize, and the uniform distribution is switched to directional distribution. directional extraction is carried out on some areas with low extraction degree, thereby dissolving the difficult-to-extract areas. When the extraction rate drops to 80-90% of the peak value, ultrasonic extraction with 75% ethanol is used to concentrate the extract. S5: Mix the volatile oil and extract, add polyethylene glycol 6000 and poloxamer, heat to 85℃ to melt, stir evenly to fully mix the agarwood extract with the matrix to obtain a medicinal solution. Place the medicinal solution in the storage tank of the pelleting machine, keep the liquid temperature at 70-80℃, select dimethyl silicone oil as the coolant, and control the coolant temperature at 5-10℃. The droplets dripped from the pelleting machine shrink and condense into pellets in the coolant. The pellets are taken out of the coolant, the surface coolant is absorbed with filter paper, and the pellets are placed in an oven at 40-50℃ to dry for 2-4 hours to remove residual coolant and moisture. Qualified pellets are screened and packaged to obtain the finished agarwood pellets.

[0017] The technical effects and advantages of this invention are as follows: 1. By switching between two modes, the fluid distribution pattern can be dynamically adjusted as the extraction process progresses to adapt to the mass transfer kinetics requirements of different extraction stages, thereby further shortening the extraction time and increasing the yield of difficult-to-extract components. Targeted adjustments have improved process efficiency.

[0018] 2. The diameter and number of holes of the exhaust pipe are smaller than the diameter of the main hole. Under the condition that the pressure of carbon dioxide gas output from the gas tank remains unchanged, the flow rate and pressure of carbon dioxide gas discharged from the exhaust pipe increase. This will improve the extraction effect by concentrating energy to impact the difficult-to-extract and locally blocked areas through directional jet. Attached Figure Description

[0019] Figure 1 This is an overall isometric view of the present invention; Figure 2 This is a structural diagram of the internal structure of the ultrasonic extraction vessel of the present invention; Figure 3 This is a structural diagram of the dynamically adjustable distributor of the present invention in uniform distribution mode; Figure 4 This is a structural diagram of the directional plate of the present invention; Figure 5This is a structural diagram of the dynamically adjustable distributor of the present invention in directional distribution mode; Figure 6 This is a connection diagram of the switching component and the distribution plate of the present invention; Figure 7 This is a structural diagram of the hydraulic component of the present invention; Figure 8 This is a structural diagram of the unidirectional device of the present invention; Figure 9 This is a structural diagram showing the separation of the unidirectional device and the ejection mechanism of the present invention; Figure 10 This is a structural diagram of the ejection mechanism lifting one-way device of the present invention.

[0020] In the picture: 1. Ultrasonic extraction tank; 2. Dynamically adjustable distributor; 21. Distributor plate; 22. Orientation plate; 221. Exhaust pipe; 3. Gas tank; 4. Switching component; 41. Switching outer pipe; 42. Switching inner pipe; 43. Locking block; 44. Limiting seat; 45. Hydraulic component; 46. Sealing plate; 5. One-way device; 51. Lower ring; 52. Upper ring; 521. Guide rod; 53. Lower seat; 54. Upper seat; 55. Side rod; 6. Ejection mechanism; 61. Ejector rod; 62. Support frame. Detailed Implementation

[0021] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0022] See Figure 1 A gas-controlled supercritical extraction device for agarwood extract, comprising: Ultrasonic extraction vessel 1 contains the agarwood extract to be extracted, forming a material bed within it. The vessel includes an internal ultrasonic generator and an ethanol concentration sensor, and is also encased in a heating jacket. The ultrasonic generator induces vibrations within the vessel, significantly enhancing mass transfer at the microscopic scale. This energy violently disturbs the fluid, interface, and cellular structure of the material at the microscopic level. The ultrasonic waves propagate in liquid carbon dioxide as longitudinal waves, creating alternating compression and rarefaction cycles. During the rarefaction cycle, liquid molecules are pulled apart, forming tiny cavitation bubbles or cavities. In the subsequent compression cycle, these cavitation bubbles are rapidly crushed and collapse, generating extremely intense localized high temperatures and pressures within a very short time and space, accompanied by strong shock waves and high-speed microjets. The shock waves propagate through the medium, causing strong microscopic convection and agitation, accelerating the penetration of the solvent into the material and the diffusion of volatile oil solutes into the liquid carbon dioxide matrix. This overcomes the mass transfer resistance in traditional extraction, significantly improving extraction efficiency and rate. This vibration disrupts any potentially fixed carbon dioxide flow channels, forcing the solvent to flow into the previously untouched agarwood extract bed, thus resolving the issue of uneven distribution. Simultaneously, it keeps the material bed loose, preventing the aggregation of fine particles and maintaining uniform permeability.

[0023] See Figure 2 The dynamic adjustable distributor 2 has one end connected to the gas tank 3 and the other end inserted into the bottom of the ultrasonic extraction tank 1. The carbon dioxide in the gas tank 3 is evenly or directionally distributed on the cross-section of the agarwood extract bed after passing through the gas distributor 2. The dynamically adjustable distributor 2 can change the carbon dioxide distribution pattern to a uniform distribution mode and a directional distribution mode: Uniform distribution pattern: (1) In the early stage of extraction, the surface components are extracted quickly and evenly; (2) During the extraction process, the ethanol content increases, the fluid polarity increases, and the viscosity may change. The dynamic adjustable distributor 2 tends to distribute more evenly to make full use of the increased solubility.

[0024] Directional distribution pattern: For areas that are difficult to extract or are locally blocked, a more penetrating "jet" pattern is formed by directional jetting, concentrating energy to impact the difficult-to-extract areas; Switching between two modes allows the fluid distribution pattern to be dynamically adjusted as the extraction process progresses, adapting to the mass transfer kinetics requirements of different extraction stages. This further shortens the extraction time and increases the yield of difficult-to-extract components. Targeted adjustments can effectively solve extraction problems.

[0025] The supercritical fluid extraction technology represents a significant leap from automation to intelligence, achieving improved process efficiency through mode switching control.

[0026] See Figures 3-5 The dynamically adjustable distributor 2 includes a distribution plate 21 that divides the interior of the ultrasonic extraction tank 1 into upper and lower chambers. The distribution plate 21 has a chamber inside, and several main holes opened on the top of the distribution plate 21 communicate with the chamber. Several directional plates 22 are also installed inside the distribution plate 21, wherein several exhaust pipes 221 opened on the top of the directional plates 22 correspond to the number and position of the main holes. The top of the distribution plate 21 is provided with a top chamber, which is connected to the main hole through a side hole. The main hole passes through the top chamber, and the carbon dioxide discharged from the top chamber can be discharged through several main holes, thereby achieving a uniform distribution function. After the directional plate 22 is raised, the exhaust pipe 221 is inserted into the main hole, and the carbon dioxide is discharged from the exhaust pipe 221 of the directional plate 22, thereby achieving a directional distribution function.

[0027] In the uniform distribution mode, the directional plate 22 does not rise; in the directional distribution mode, the directional plate 22 in the designated area rises to achieve directional jet.

[0028] In order to enable the directional plate 22 to be raised and lowered, a cylinder is provided. The directional plate 22 is driven to move by the cylinder in the cavity. The number of cylinders is the same as the number of directional plates 22.

[0029] In order to prevent carbon dioxide from flowing into the chamber from the main hole in the uniform distribution mode, and to ensure that the gas discharged from the exhaust pipe 221 in the directional mode can be discharged from the main hole without flowing to the side hole, a one-way device 5 is provided. See Figures 8-10 Specifically, a one-way device 5 is installed in the main hole below the top chamber. The one-way device 5 includes a lower ring 51, an upper ring 52, a lower seat 53, an upper seat 54, and a side rod 55. The lower ring 51 is fixed to the bottom of the main hole, and the lower seat 53 is fixed on the lower ring 51. Both the lower seat 53 and the lower ring 51 have through holes. The upper ring 52 is sealed to the main hole. The guide rod 521 fixed at the bottom of the upper ring 52 is inserted into the lower seat 53. The upper ring 52 and the lower seat 53 are also connected by a spring. The inner circumferential surface of the upper ring 52 is connected to the upper seat 54 via the side rod 55, forming a gas channel between the upper ring 52 and the upper seat 54. The upper seat 54 is used to seal or open the lower hole.

[0030] Specifically, the lower ring 51 and lower seat 53 are fixed in position, while the upper ring 52 and upper seat 54 are movable. The guide rod 521 fixed on the upper ring 52 is inserted into the lower seat 53. The upper ring 52 slides up and down along the lower seat 53. With the help of the spring structure, the bottom end of the upper seat 54 is inserted into the lower hole of the lower seat 53 without the action of external force, thereby sealing the bottom end of the main hole below the side hole. The agarwood material falls into the cavity from the main hole. As the pressure in the cavity increases, the pressure will act on the upper seat 54, further increasing the pressure between the upper seat 54 and the lower seat 53, thereby maintaining the seal.

[0031] In order to ensure that when the exhaust pipe 221 is inserted into the main hole when switching to the directional distribution mode, the one-way device 5 will not affect its ventilation, and the one-way device 5 can also be used to block the side hole, an ejection mechanism 6 is provided. Specifically, an ejector mechanism 6 is mounted on the top of the exhaust pipe 221. The ejector mechanism 6 includes an ejector rod 61 and a support frame 62. The ejector rod 61 is fixed to the exhaust pipe 221 by the support frame 62. The exhaust pipe 221 moves upward through the lower hole, the push rod 61 first contacts the upper seat 54 and then pushes the upper ring 52 to move upward along the main hole and is used to seal the side hole. The carbon dioxide in the gas tank 3 is discharged into the ultrasonic extraction tank 1 through the gas channel.

[0032] In order to allow carbon dioxide gas to be discharged from the directional plate 22 or the distribution plate 21 under different mode switching, a switching component 4 is provided, which is used to connect the gas tank 3 with the distribution plate 21 or the directional plate 22. The switching function is achieved by the directional plate 22 moving up and down in the chamber. When several directional plates 22 do not move upward, the carbon dioxide discharged from the gas tank 3 is discharged from the main hole of the distribution plate 21 and evenly distributed on the agarwood extract bed. When one of the directional plates 22 moves upward, the exhaust pipe 221 is inserted into the main hole, and the carbon dioxide discharged from the gas tank 3 is directionally distributed on the agarwood extract bed.

[0033] See Figures 5-7 Specifically, the switching component 4 includes a switching outer tube 41, a switching inner tube 42, a locking block 43, a limiting seat 44, a hydraulic component 45, and a sealing plate 46. The switching outer tube 41 and the switching inner tube 42 are concentrically arranged in the chamber, wherein the switching inner tube 42 is connected to the top chamber and the gas tank 3. The number of limiting seats 44 is the same as that of the directional plates 22. The limiting seats 44 are fixed on the outer wall of the switching inner tube 42. The secondary hole 1 opened on the limiting seat 44 is connected to the switching inner tube 42. The directional plate 22 is connected to one end of the locking block 43. The other end of the locking block 43 passes through the strip groove of the switching outer tube 41 and is locked on the limiting seat 44. The secondary hole 2 opened on the locking block 43 is connected to the inner cavity of the directional plate 22. The exhaust pipe 221 is also connected to the inner cavity. Hydraulic component 45 is installed inside switching inner tube 42, and hydraulic component 45 is connected to sealing plate 46.

[0034] See Figure 7 The hydraulic component 45 consists of two sets of hydraulic chambers, one end of which is connected to the locking block 43 and the other end is connected to the sealing plate 46. When the locking block 43 moves upward, it drives the sealing plate 46 to move upward as well. The sealing plate 46 can block the hole of the switching inner tube 42. When the locking block 43 moves downward, it drives the switch to move downward, opening the hole of the switching inner tube 42.

[0035] When the directional plate 22 moves upward for directional distribution, the hydraulic component 45 drives the sealing plate 46 to seal the switching inner tube 42, and the secondary hole one and secondary hole two are connected.

[0036] The cylinder drives the directional plate 22 at the corresponding blocked or difficult-to-extract area projection to move upward. The push rod 61 of the exhaust pipe 221 first contacts the upper seat 54 and then pushes the upper ring 52 to move upward along the main hole. During the upward movement of the directional plate 22, the locking block 43 also slides along the limit seat 44, driving the hydraulic component 45 to move synchronously along the switching inner tube 42, achieving three purposes: First: The exhaust pipe 221 moves upward and enters the main hole, and lifts the upper seat 54 from the lower seat 53. The upper ring 52 blocks the side hole, and the exhaust pipe 221 is connected to the pre-emptive tank chamber through the gas passage. Second: The hydraulic component 45 moves the drive plate 46 to seal the switching inner tube 42, preventing carbon dioxide from flowing into the top chamber from the switching inner tube 42. Combined with the upper ring 52 to block the side hole, it further improves its sealing performance. Third: The secondary hole 2 on the card block 43 is connected to the inner cavity of the directional plate 22, and the secondary hole 1 and the secondary hole 2 are connected. At this time, the carbon dioxide in the gas tank 3 first flows into the switching inner tube 42, then flows into the directional plate 22 along the secondary hole 1 and the secondary hole 2, and then is discharged into the ultrasonic extraction tank 1 through the exhaust pipe 221.

[0037] The circular hole at the center of the distribution plate 21 can be fitted with a valve that can be opened and closed as needed, and can be independently controlled in directional jet mode and distribution mode.

[0038] Because the diameter and number of holes of the exhaust pipe 221 are smaller than the diameter of the main hole, the flow rate and pressure of the carbon dioxide gas discharged from the exhaust pipe 221 increase when the pressure of the carbon dioxide gas output from the gas tank 3 remains unchanged. This increases the extraction efficiency by using directional jets to concentrate energy on the difficult-to-extract and locally blocked areas.

[0039] Different modes can be switched according to different extraction levels, and the directional distribution area is adjustable, which can be adjusted in a timely manner according to different needs. The extraction method can be dynamically adjusted according to the conditions inside the tank.

[0040] An extraction process for agarwood extract includes the following steps: S1: Processing of Agarwood Raw Materials: S11: Raw material selection: Select agarwood blocks of consistent quality; S12: Crushing process: Use a dedicated crusher to crush the material, then pass it through a 20-40 mesh sieve; S13: Moisture control: Adjust the moisture content to 8-12%; S2: Extraction tank filling: S21: Distributor check: Confirm that the adjustable distributor is fully open; S22: Layered filling: Layered compaction filling method is adopted; S23: Filling height: Control the filling height to 70-80% of the effective height of the extraction vessel; S3: Control parameter initialization: S31: The distributor is set to uniform distribution; S4: Extraction S41: The extraction tank is pressurized to 25-35 MPa and the temperature is increased to 40-50℃. The carbon dioxide flow rate is 20-30 L / h, the ethanol concentration is 70%-80%, and the material-liquid ratio is 1:10-1:15. Combined with ultrasonic-assisted ethanol extraction of non-volatile components, the ultrasonic power is 300W and the time is 30min. The distributor is used in a uniform distribution mode to extract volatile oil. S42: Mode switching: When the extraction rate drops to 60-70% of the peak value, the bed pressure drop tends to stabilize, and the uniform distribution is switched to directional distribution. directional extraction is carried out on some areas with low extraction degree, thereby dissolving the difficult-to-extract areas. When the extraction rate drops to 80-90% of the peak value, ultrasonic extraction with 75% ethanol is used to concentrate the extract. S5: Mix the volatile oil and extract, add polyethylene glycol 6000 and poloxamer, heat to 85℃ to melt, stir evenly to fully mix the agarwood extract with the matrix to obtain a medicinal solution. Place the medicinal solution in the storage tank of the pelleting machine, keep the liquid temperature at 70-80℃, select dimethyl silicone oil as the coolant, and control the coolant temperature at 5-10℃. The droplets dripped from the pelleting machine shrink and condense into pellets in the coolant. The pellets are taken out of the coolant, the surface coolant is absorbed with filter paper, and the pellets are placed in an oven at 40-50℃ to dry for 2-4 hours to remove residual coolant and moisture. Qualified pellets are screened and packaged to obtain the finished agarwood pellets.

[0041] Polyethylene glycol 6000 and poloxamer were used as the matrix.

[0042] Excellent formability: By selecting a suitable matrix and optimizing the dripping process parameters, the formability of the pellets is significantly improved. The matrix has good solubility and plasticity, which allows the medicine to be smoothly formed during the dripping process, resulting in smooth, round pellets without adhesion.

[0043] Short dispersibility time: The freeze-drying method for preparing agarwood extract maximizes the retention of its active ingredients, and the fine particle size of the extract allows for faster dispersibility when mixed with the matrix. Simultaneously, the added antioxidants and plasticizers help improve the physical properties of the pellets, further shortening the dispersibility time and enabling faster drug release and absorption, thus improving bioavailability.

[0044] Stable content of active ingredients: During the extraction process, ethanol reflux extraction is used, and processes such as vacuum concentration and freeze-drying minimize the loss of active ingredients. Antioxidants added during production prevent oxidation and deterioration of the active ingredients, ensuring product quality stability.

[0045] The following are specific examples: Example 1: Preparation of agarwood extract Take 1000g of agarwood, grind it into coarse powder, and pass it through a 20-mesh sieve.

[0046] Place the coarse agarwood powder in an extraction tank, add 8 times the volume of 60% ethanol, soak for 1 hour, then heat and reflux to extract twice, 1 hour each time.

[0047] Combine the extracts, filter, and concentrate the filtrate under reduced pressure to obtain a clear extract with a relative density of 1.10 (measured at 60℃).

[0048] The extract was placed in a freeze dryer and pre-frozen at -40°C for 2 hours, and then sublimated and dried under a vacuum of 10 Pa for 10 hours to obtain 120g of agarwood extract.

[0049] 2. Selection and treatment of the substrate

[0050] Weigh out 360g of polyethylene glycol 6000 and 120g of poloxamer 188, mix them together, place them in a heating container, heat and melt them at 70℃, and stir until uniform.

[0051] 3. Preparation of the medicinal solution

[0052] Agarwood extract is added to the molten matrix and stirred until homogeneous to obtain the medicinal solution.

[0053] Add 0.48g of vitamin E and 4.8g of glycerin to the solution and continue stirring for 15 minutes.

[0054] 4. Drip

[0055] Place the medicine solution in the storage tank of the pelleting machine and keep the temperature of the medicine solution at 70℃.

[0056] Dimethyl silicone oil was selected as the coolant, and the coolant temperature was controlled at 5℃.

[0057] Adjust the inner diameter of the dropper head of the pellet mill to 2mm, the drop distance to 5cm, and the drop speed to 30 drops / minute for pelleting.

[0058] 5. Post-processing

[0059] Remove the pellets from the coolant and use filter paper to absorb the coolant from their surface.

[0060] The pellets were dried in an oven at 40°C for 2 hours.

[0061] After selecting qualified agarwood pellets, they are packaged to obtain the finished agarwood pellet product.

[0062] Example 2

[0063] Preparation of agarwood extract

[0064] Take 1000g of agarwood, grind it into coarse powder, and pass it through a 30-mesh sieve.

[0065] Place the coarse agarwood powder in an extraction tank, add 10 times the volume of 70% ethanol, soak for 2 hours, then heat and reflux to extract twice, each time for 1.5 hours.

[0066] Combine the extracts, filter, and concentrate the filtrate under reduced pressure to obtain a clear extract with a relative density of 1.15 (measured at 60℃).

[0067] The extract was placed in a freeze dryer and pre-frozen at -30°C for 3 hours, and then sublimated and dried under a vacuum of 20 Pa for 15 hours to obtain 130g of agarwood extract.

[0068] 2. Selection and treatment of the substrate

[0069] Weigh out 520g of polyethylene glycol 6000 and 130g of poloxamer 188, mix them together, place them in a heating container, heat and melt them at 75°C, and stir until uniform.

[0070] 3. Preparation of the medicinal solution

[0071] Agarwood extract is added to the molten matrix and stirred until homogeneous to obtain the medicinal solution.

[0072] Add 0.975g of vitamin E and 19.5g of glycerin to the solution and continue stirring for 20 minutes.

[0073] 4. Drip

[0074] Place the medicine solution in the storage tank of the pelleting machine and keep the temperature of the medicine solution at 75℃.

[0075] Dimethyl silicone oil was selected as the coolant, and the coolant temperature was controlled at 8℃.

[0076] Adjust the inner diameter of the dropper head of the pellet mill to 2.5mm, the drop distance to 7cm, and the drop speed to 40 drops / minute for pelleting.

[0077] 5. Post-processing

[0078] Remove the pellets from the coolant and use filter paper to absorb the coolant from their surface.

[0079] The pellets were dried in an oven at 45°C for 3 hours.

[0080] After selecting qualified agarwood pellets, they are packaged to obtain the finished agarwood pellet product.

[0081] Example 3

[0082] 1. Preparation of Agarwood Extract

[0083] Take 1000g of agarwood, grind it into coarse powder, and pass it through a 40-mesh sieve.

[0084] Place the coarse agarwood powder in an extraction tank, add 12 times the volume of 80% ethanol, soak for 3 hours, then heat and reflux to extract 3 times, 2 hours each time.

[0085] Combine the extracts, filter, and concentrate the filtrate under reduced pressure to obtain a clear extract with a relative density of 1.20 (measured at 60℃).

[0086] The extract was placed in a freeze dryer and pre-frozen at -20°C for 4 hours, and then sublimated and dried under a vacuum of 30 Pa for 20 hours to obtain 140g of agarwood extract.

[0087] 2. Selection and treatment of the substrate

[0088] Weigh out 6000560g of polyethylene glycol and 140g of poloxamer 188, mix them together, place them in a heating container, heat and melt them at 80℃, and stir until uniform.

[0089] 3. Preparation of the medicinal solution

[0090] Agarwood extract is added to the molten matrix and stirred until homogeneous to obtain the medicinal solution.

[0091] Add 2.1g of vitamin E and 21g of glycerin to the solution and continue stirring for 30 minutes.

[0092] 4. Drip

[0093] Place the medicine solution in the storage tank of the pelleting machine and keep the temperature of the medicine solution at 80℃.

[0094] Dimethyl silicone oil was selected as the coolant, and the coolant temperature was controlled at 10℃.

[0095] Adjust the inner diameter of the dropper head of the pellet mill to 3mm, the drop distance to 10cm, and the drop speed to 60 drops / minute for pellet production.

[0096] 5. Post-processing

[0097] Remove the pellets from the coolant and use filter paper to absorb the coolant from their surface.

[0098] The pellets were dried in an oven at 50°C for 4 hours.

[0099] After selecting qualified agarwood pellets, they are packaged to obtain the finished agarwood pellet product.

[0100] By optimizing the preparation process of agarwood extract, selecting suitable matrices and excipients, and strictly controlling the dripping process parameters, the produced agarwood dripping pills exhibit good formability, short dissolution time, and stable content of active ingredients. Compared with existing technologies, this method has significant advantages, improving the bioavailability and clinical efficacy of agarwood and showing promising market application prospects. Furthermore, the production method of this invention is simple to operate and easy to industrialize, providing reliable technical support for the large-scale production of agarwood dripping pills.

[0101] Finally, it should be noted that the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A gas-controlled supercritical extraction device for agarwood extract, characterized in that, include: An ultrasonic extraction vessel (1) contains the agarwood extract to be extracted, and the agarwood extract forms a material bed within the ultrasonic extraction vessel (1); The dynamic adjustable distributor (2) is connected at one end to the gas tank (3) and the other end is inserted into the bottom of the ultrasonic extraction tank (1). The carbon dioxide in the gas tank (3) is evenly or directionally distributed on the cross-section of the agarwood extract bed after passing through the gas distributor (2). The dynamically adjustable distributor (2) includes a distribution plate (21) that divides the interior of the ultrasonic extraction tank (1) into upper and lower chambers. The distribution plate (21) has a chamber inside, and several main holes opened on the top of the distribution plate (21) are connected to the chamber. Several directional plates (22) are also installed inside the distribution plate (21), and several exhaust pipes (221) opened on the top of the directional plates (22) correspond to the number and position of the main holes. The switching component (4) is used to connect the gas tank (3) with the distribution plate (21) or the directional plate (22). It achieves the switching function by moving up and down in the chamber through the directional plate (22). If none of the directional plates (22) move upward, the carbon dioxide discharged from the gas tank (3) will be discharged from the main hole of the distribution plate (21) and evenly distributed on the agarwood extract bed. When one of the directional plates (22) moves upward, the exhaust pipe (221) is inserted into the main hole, and the carbon dioxide discharged from the gas tank (3) is directionally distributed on the agarwood extract bed.

2. The gas-controlled supercritical extraction equipment for agarwood extract according to claim 1, characterized in that, The ultrasonic extraction tank (1) has a built-in ultrasonic generator and an ethanol concentration sensor, and the ultrasonic extraction tank (1) is also covered with a heating jacket.

3. The gas-controlled supercritical extraction equipment for agarwood extract according to claim 2, characterized in that, The top of the distribution plate (21) is provided with a top chamber, wherein the top chamber is connected to the main hole through a side hole, and a one-way device (5) is installed in the main hole below the top chamber.

4. The gas-controlled supercritical extraction equipment for agarwood extract according to claim 3, characterized in that, The one-way device (5) includes a lower ring (51), an upper ring (52), a lower seat (53), an upper seat (54), and a side rod (55). The lower ring (51) is fixed to the bottom of the main hole, and the lower seat (53) is fixed on the lower ring (51). Both the lower seat (53) and the lower ring (51) have through holes. The upper ring (52) is sealed to the main hole. The guide rod (521) fixed at the bottom of the upper ring (52) is inserted into the lower seat (53). The upper ring (52) and the lower seat (53) are also connected by a spring. The inner circumferential surface of the upper ring (52) is connected to the upper seat (54) through the side rod (55), and a gas channel is formed between the upper ring (52) and the upper seat (54). The upper seat (54) is used to seal or open the lower hole.

5. The gas-controlled supercritical extraction equipment for agarwood extract according to claim 4, characterized in that, The exhaust pipe (221) is equipped with an ejector mechanism (6), which includes a push rod (61) and a support frame (62). The push rod (61) is fixed to the exhaust pipe (221) by the support frame (62).

6. The gas-controlled supercritical extraction equipment for agarwood extract according to claim 5, characterized in that, The exhaust pipe (221) moves upward through the lower hole, the push rod (61) first contacts the upper seat (54) and then pushes the upper ring (52) to move upward along the main hole and is used to seal the side hole. The carbon dioxide in the gas tank (3) is discharged into the ultrasonic extraction tank (1) through the gas channel.

7. The gas-controlled supercritical extraction equipment for agarwood extract according to claim 6, characterized in that, The switching component (4) includes a switching outer tube (41), a switching inner tube (42), a locking block (43), a limiting seat (44), a hydraulic component (45), and a sealing plate (46). The switching outer tube (41) and the switching inner tube (42) are concentrically arranged in the chamber, wherein the switching inner tube (42) is connected to the top chamber and the gas tank (3). The number of slots in the limiting seat (44) is the same as that in the directional plate (22). The limiting seat (44) is fixed on the outer wall of the switching inner tube (42). The secondary hole one opened on the limiting seat (44) is connected to the switching inner tube (42). The directional plate (22) is connected to one end of the card block (43). The other end of the card block (43) passes through the strip groove of the switching outer tube (41) and is locked in the slot of the limiting seat (44). The secondary hole two opened on the card block (43) is connected to the inner cavity of the directional plate (22). The exhaust pipe (221) is also connected to the inner cavity. The hydraulic component (45) is installed on the switching inner tube (42), and the hydraulic component (45) is connected to the sealing plate (46).

8. The gas-controlled supercritical extraction equipment for agarwood extract according to claim 7, characterized in that, When the directional plate (22) moves upward for directional distribution, the hydraulic component (45) drives the sealing plate (46) to seal the switching inner tube (42), and the secondary hole one and secondary hole two are connected.

9. The gas-controlled supercritical extraction equipment for agarwood extract according to claim 8, characterized in that, The orientation plate (22) is driven to move by cylinders inside the chamber, and the number of cylinders is the same as the number of orientation plates (22).

10. An extraction process for agarwood extract, applied to the supercritical extraction equipment described in claim 9, characterized in that: Includes the following steps: S1: Processing of Agarwood Raw Materials: S11: Raw material selection: Select agarwood blocks of consistent quality; S12: Crushing process: Use a dedicated crusher to crush the material, then pass it through a 20-40 mesh sieve; S13: Moisture control: Adjust the moisture content to 8-12%; S2: Extraction tank filling: S21: Distributor check: Confirm that the adjustable distributor is fully open; S22: Layered filling: Layered compaction filling method is adopted; S23: Filling height: Control the filling height to 70-80% of the effective height of the extraction vessel; S3: Control parameter initialization: S31: The distributor is set to uniform distribution; S4: Extraction S41: The extraction tank is pressurized to 25-35 MPa and the temperature is increased to 40-50℃. The carbon dioxide flow rate is 20-30 L / h, the ethanol concentration is 70%-80%, and the material-liquid ratio is 1:10-1:

15. Combined with ultrasonic-assisted ethanol extraction of non-volatile components, the ultrasonic power is 300W and the time is 30min. The distributor is used in a uniform distribution mode to extract volatile oil. S42: Mode switching: When the extraction rate drops to 60-70% of the peak value, the bed pressure drop tends to stabilize, and the uniform distribution is switched to directional distribution. directional extraction is carried out on some areas with low extraction degree, thereby dissolving the difficult-to-extract areas. When the extraction rate drops to 80-90% of the peak value, ultrasonic extraction with 75% ethanol is used to concentrate the extract. S5: Mix the volatile oil and extract, add polyethylene glycol 6000 and poloxamer, heat to 85℃ to melt, stir evenly to fully mix the agarwood extract with the matrix to obtain a medicinal solution. Place the medicinal solution in the storage tank of the pelleting machine, keep the liquid temperature at 70-80℃, select dimethyl silicone oil as the coolant, and control the coolant temperature at 5-10℃. The droplets dripped from the pelleting machine shrink and condense into pellets in the coolant. The pellets are taken out of the coolant, the surface coolant is absorbed with filter paper, and the pellets are placed in an oven at 40-50℃ to dry for 2-4 hours to remove residual coolant and moisture. Qualified pellets are screened and packaged to obtain the finished agarwood pellets.

Images