Separating device

Abstract

The invention relates to the field of beverage processing, and discloses a separation device which comprises a separation barrel, a gas conveying pipe is installed at the bottom of the separation barrel, a cover plate is installed at the top of the separation barrel, and the gas conveying pipe is used for conveying supercritical carbon dioxide into the separation barrel; and the moving plate is installed in the separation barrel, a collecting groove is formed in the bottom of the moving plate, a first elastic piece is installed between the moving plate and the cover plate, and the moving plate is arranged to move upwards under the pressure effect of supercritical carbon dioxide so as to prolong the layering time of supercritical carbon dioxide and sulfide. According to the device, the moving plate slowly ascends through elastic supporting of the first elastic piece, the flowing time of supercritical carbon dioxide in the separation barrel is prolonged, it is ensured that sulfide fully floats upwards and is enriched in the collecting groove due to density difference, the opening area of the collecting holes is dynamically adjusted through the control head, and directional efficient recovery of the tea polyphenol phase is achieved.

Description

Technical Field

[0001] The present invention relates to the field of beverage processing, and particularly to a separation device. Background Art

[0002] The tea polyphenols in tea polyphenol-containing beverages mainly come from tea leaves. During the production and processing of tea polyphenol beverages, it is necessary to extract the tea polyphenols from the tea leaves. As agricultural crops, the fertilizers such as ammonium sulfate and superphosphate used in the planting stage of tea leaves contain sulfates. Excessive use will cause the sulfur in the soil to exceed the standard. Some fungicides (such as sulfur suspension agents) are directly sprayed on the tea leaves, resulting in surface sulfur residues. Low-quality tea leaves will further generate organic sulfur compounds such as thioamino acids due to microbial metabolism or incomplete high-temperature fixation during the processing. Supercritical CO2 fluid extraction (SFE) is a chemical reaction that utilizes the relationship between the solubility of supercritical fluids and their density, that is, the influence of pressure and temperature on the solubility of supercritical fluids. Supercritical CO 2 During the operation of the extraction equipment, if the tea leaves contain sulfides (such as hydrogen sulfide or other sulfur-containing compounds), if these sulfides cannot be separated and collected, they may react with CO 2 to form thiocarbonates under high pressure.

[0003] After retrieval, the publication number CN108948101A discloses a method for ultrasonic supercritical combined extraction of tea polyphenols. The method for ultrasonic supercritical combined extraction of tea polyphenols includes steps such as raw material treatment, ultrasonic treatment, supercritical CO2 extraction, separation and purification, etc. Using the above method to extract tea polyphenols can improve the extraction rate and purity of tea polyphenols.

[0004] The existing separation devices rely on post-filtering or adsorption units to separate sulfides, but thiocarbonates are prone to clogging valves during the extraction stage, and it is impossible to synchronously separate and collect sulfides during the process of extracting and separating tea polyphenols. Summary of the Invention

[0005] In order to solve the problem that the existing separation devices rely on post-filtering or adsorption units to separate sulfides, but thiocarbonates are prone to clogging valves during the extraction stage, and it is impossible to synchronously separate and collect sulfides during the process of extracting and separating tea polyphenols, the present invention is achieved through the following technical solutions.

[0006] On the one hand, the present invention discloses a beverage containing tea polyphenols, including the following components in mass percentages: 0.15% - 0.4% tea polyphenols, 0.03% - 0.08% chitosan, 0.03% - 0.07% vitamin E, 0.02% - 0.05% bamboo leaf antioxidants, 2% - 4% fructooligosaccharide, 0.0005% - 0.0015% mogroside, 0.12% - 0.18% stabilizer, 0.12% - 0.25% malic acid, and the balance deionized water; The chitosan forms hydrogen bonds with tea polyphenols through the amino groups in its molecular structure and adsorbs metal ions in the drink through positive charges.

[0007] Preferably, the stabilizer is composed of gellan gum and hydroxypropyl methylcellulose, and the mass ratio of gellan gum to hydroxypropyl methylcellulose is 1:1.5.

[0008] On the other hand, the present invention also discloses a separation device, including: A separation barrel, with an air delivery pipe installed at the bottom of the separation barrel and a cover plate installed at the top. The air delivery pipe is used to deliver supercritical carbon dioxide into the separation barrel; A moving plate, installed inside the separation barrel. A collection groove is opened at the bottom of the moving plate. A first elastic member is installed between the moving plate and the cover plate. The moving plate is arranged to move upward under the action of the supercritical carbon dioxide pressure to extend the stratification time of the supercritical carbon dioxide and sulfide; A first collection pipe, with both ends respectively penetrating through the cover plate and the separation barrel. Collection holes are opened on the first collection pipe for collecting the supercritical fluid phase after dissolving tea polyphenols; A second collection pipe, installed on the moving plate, with one end extending into the collection groove for collecting sulfide when the moving plate moves to the top area of the separation barrel; A first piston head, installed inside the second collection pipe. The first piston head is driven by a control mechanism to adsorb sulfide in the collection groove.

[0009] Preferably, the first collection pipe includes: A control head, installed inside the first collection pipe, covering the collection holes; A second elastic member, with one end installed on the control head and the other end installed on the top wall of the first collection pipe; A control rod, installed at the top end of the control head. A ventilation hole is opened on the cover plate. One end of the control rod extends to the outside of the first collection pipe and passes through the ventilation hole and is placed inside the separation barrel; A connection head, installed on the control rod. The connection head is provided with a telescopic groove. The control rod is connected in the telescopic groove. When the moving plate moves upward, it first pushes the connection head into the ventilation hole and blocks the ventilation hole until the bottom wall of the telescopic groove contacts the end of the control rod. The connection head drives the control rod to move upward, and the control head opens the collection holes to collect the supercritical fluid phase rich in tea polyphenols.

[0010] Preferably, the control mechanism includes: A connecting pipe, which is disposed in the second collecting pipe and has one end extending outside the connecting pipe; A second piston head is installed in the connecting pipe; A moving rod, one end of which is connected to the second piston head, and the other end of which is connected to the first piston head; When the connecting head blocks the vent hole, the air pressure between the moving plate and the cover plate increases, pushing the second piston head to move in the connecting tube, and driving the first piston head to move in the second collecting tube through the moving rod to adsorb sulfide.

[0011] Preferably, the control mechanism comprises a first power source installed on the second collecting tube, and a power shaft of the first power source is connected to the first piston head for controlling the movement of the first piston head in the second collecting tube.

[0012] Preferably, a first one-way valve is installed at the gas inlet of the second collecting pipe, and the first one-way valve is configured to only allow gas to flow from the collecting tank into the second collecting pipe in one direction.

[0013] Preferably, a valve is installed on the second collecting pipe for discharging the collected sulfide after opening.

[0014] Preferably, it also includes a stirring component installed on the movable plate and used for stirring the raw materials.

[0015] Preferably, the stirring assembly comprises: A connecting sleeve, which is movably mounted on the first collecting tube and is rotatably connected to the moving plate; A stirring rod is installed on the connecting sleeve; The movable groove is opened on the outer surface of the first collecting tube and is spiral-shaped. The stirring rod cooperates with the movable groove through the movable block, so that when the movable plate rises, the stirring rod is driven to rotate around the first collecting tube and stir the raw materials.

[0016] The present invention provides a separation device. Compared with the prior art, the device has the following beneficial effects: the moving plate slowly rises through the elastic support of the first elastic member, prolonging the flow time of the supercritical carbon dioxide in the separation barrel, ensuring that the sulfide fully floats up and is enriched in the collection tank due to the density difference, the vent hole is closed when the moving plate rises, forming a closed high-pressure environment, forcing the sulfide to stay in the collection tank, and dynamically adjusting the opening area of ​​the collection hole through the control head to achieve directional and efficient recovery of the tea polyphenol phase.

[0017] The second collecting tube rises synchronously with the moving plate to the top of the separation barrel. The one-way valve at its air inlet ensures the one-way inflow of sulfide. When the moving plate closes the vent, the increased air pressure in the barrel drives the piston head to adsorb sulfide and discharge it directly through the second collecting tube, avoiding the deposition of thiocarbonate in valves or pipes.

[0018] When the moving plate rises, it drives the stirring rod to rotate through the spiral groove, forcibly breaks the raw materials, enhances the contact efficiency between supercritical carbon dioxide and the materials, and improves the extraction rate of tea polyphenols. The separation of sulfides and the collection of tea polyphenols are completed in stages through the same device, reducing the efficiency loss caused by the switching of multiple devices in the traditional process.

[0019] Stabilize the molecular structure of tea polyphenols through hydrogen bonding, effectively delaying oxidation; at the same time, utilize the positive charge characteristics to adsorb metal ions in the beverage, preventing metal ions from complexing with tea polyphenols to form precipitates; The combination of vitamin E and bamboo leaf antioxidants forms an antioxidant network covering both the oil and water phases, significantly enhancing the free radical scavenging ability of the beverage.

[0020] Fructooligosaccharides provide a mild sweetness and weaken the astringency, and mogroside precisely adjusts the sweetness, avoiding the health hazards of high sugar or artificial sweeteners. At the same time, it improves the palatability of the beverage. Fructooligosaccharides promote intestinal health, and malic acid coordinates the flavor, forming a beverage system with both functionality and natural flavor. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 It is a schematic diagram of the three-dimensional structure proposed by the present invention.

[0022] Figure 2 It is a schematic diagram of the cross-section of the separation barrel proposed by the present invention.

[0023] Figure 3 It is a schematic diagram of the structures of the separation barrel, moving plate, cover plate and first collection pipe proposed by the present invention.

[0024] Figure 4 It is a schematic diagram of the cross-section of the moving plate, cover plate, first collection pipe and second collection pipe proposed by the present invention.

[0025] Figure 5 It is a schematic diagram of the cross-section of the moving plate, first collection pipe, control rod and connector proposed by the present invention.

[0026] Figure 6 It is a schematic diagram of the structures of the moving plate, first collection pipe, stirring rod, connecting sleeve and moving block proposed by the present invention.

[0027] Figure 7 It is a schematic diagram of the structures of the control head, control rod and connector proposed by the present invention.

[0028] Figure 8 It is a schematic diagram of the structures of the second collection pipe, connecting pipe and valve nozzle proposed by the present invention.

[0029] Figure 9 It is a schematic diagram of the cross-section of the second collection pipe and connecting pipe proposed by the present invention.

[0030] Figure 10 It is a schematic diagram of the control mechanism of Example 5.

[0031] Figure 11 It is a schematic structural diagram of the stirring assembly in Example 5.

[0032] Figure 12 It is a data table for stability detection.

[0033] Figure 13 It is a data table for taste evaluation.

[0034] Figure 14 It is a data table for rheological properties.

[0035] Figure 15 It is a data table for microorganism detection.

[0036] The reference numerals in the figure are as follows: 100, separation barrel; 101, gas transmission pipe; 200, moving plate; 201, collection tank; 202, first one-way valve; 203, first elastic member; 300, cover plate; 301, ventilation hole; 400, first collection pipe; 401, collection hole; 402, control head; 403, second elastic member; 404, control rod; 405, connection head; 500, second collection pipe; 501, connecting pipe; 502, valve nozzle; 503, first piston head; 504, moving rod; 505, second piston head; 506, first power source; 600, stirring rod; 601, connecting sleeve; 602, moving block; 603, moving groove; 604, second power source. Specific embodiments

[0037] The present invention will be further described below in conjunction with specific embodiments. It should be understood that these embodiments are only used to illustrate the present invention and not to limit the protection scope of the present invention.

[0038] The following illustrates the implementation manners of the present invention through specific specific examples. Those skilled in the art can easily understand other advantages and effects of the present invention from the content disclosed in this specification. The present invention can also be implemented or applied through other different specific implementation manners. Various details in this specification can also be modified or changed based on different viewpoints and applications without departing from the spirit of the present invention.

[0039] Example 1: A tea polyphenol-containing beverage, comprising the following components in mass percentage: tea polyphenols 0.3%, chitosan 0.05%, vitamin E 0.05%, bamboo leaf antioxidant 0.035%, fructooligosaccharide 3%, mogroside 0.001%, stabilizer 0.15%, malic acid 0.18%, and the balance deionized water; wherein, the chitosan forms a hydrogen bond with the tea polyphenols through the amino group in the molecular structure, and adsorbs metal ions in the beverage through positive charges to inhibit the oxidation of tea polyphenols and the complex precipitation of metal ions.

[0040] The stabilizer is composed of gellan gum and hydroxypropyl methylcellulose, and the mass ratio of gellan gum to hydroxypropyl methylcellulose is 1:1.5.

[0041] As the core functional component, tea polyphenols can not only ensure that the beverage has significant health care functions such as antioxidant and antibacterial effects, but also effectively control the bitter taste within an acceptable range through the subsequent taste improvement components.

[0042] Among the common beverage components, chitosan is usually used as a flocculant for processes such as fruit juice clarification, and realizes liquid clarification by adsorbing suspended particles. However, in this solution, after chitosan is combined with other components, it plays unique and non-obvious multiple roles: on the one hand, the amino group in the chitosan molecular structure can form a hydrogen bond with the tea polyphenol molecule to stabilize the tea polyphenol structure and inhibit its oxidation; on the other hand, chitosan has a positive charge and can undergo electrostatic adsorption with negatively charged metal ions (such as iron ions and copper ions) in fruit juice to prevent metal ions from reacting with tea polyphenols, thereby solving the precipitation problem. In addition, chitosan can also form an extremely thin protective film on the surface of the beverage to isolate oxygen and further improve the stability of the beverage. Its addition amount is controlled within 0.03%-0.08%. Within this range, it can play a stabilizing role without having a negative impact on the taste and fluidity of the beverage.

[0043] For the antioxidant synergistic combination, vitamin E and bamboo leaf antioxidant are compounded. Vitamin E is a fat-soluble antioxidant that can play an antioxidant role at the oil-water interface of the beverage to prevent oil oxidation and rancidity; bamboo leaf antioxidant is rich in components such as flavonoids and lactones and has the ability to efficiently scavenge free radicals. It acts synergistically with tea polyphenols to form a water-soluble and fat-soluble antioxidant dual system.

[0044] Fructooligosaccharide and mogroside are selected for compounding. Fructooligosaccharide can not only provide a mild sweetness, but also promote the proliferation of beneficial bacteria in the intestine and has certain health care functions; mogroside has a very high sweetness (about 300-400 times that of sucrose) and almost no calories. The combination of the two can accurately adjust the sweetness, and at the same time, the presence of fructooligosaccharide can weaken the astringency of tea polyphenols.

[0045] The stabilizer is a compound of gellan gum and hydroxypropyl methylcellulose (HPMC). Gellan gum can form a transparent and tough gel network in the presence of divalent cations, which can effectively encapsulate tea polyphenols and other unstable components; HPMC has good film-forming property and thickening property. The compounding ratio of the two is 1:1.5, and the total content is controlled at 0.12% - 0.18%. It can maintain the uniform and stable state of the drink during high-temperature sterilization and long-term storage, and prevent stratification and precipitation.

[0046] Malic acid is selected as the acidulant. The mild acidity of malic acid can better coordinate with other sweet and astringent components, enhancing the richness of the taste; trace amounts of minerals such as zinc and magnesium can be added according to requirements, with the total content not exceeding 0.008%, to enhance the nutritional value of the drink.

[0047] The addition of chitosan solves problems such as protein denaturation, tea polyphenol precipitation, and blockage of pipelines by sodium alginate gel; the new stabilizer combination enables the drink to maintain good fluidity and uniformity during the processing process, improving production efficiency.

[0048] Example 2: A drink containing tea polyphenols, including the following components in mass percentage: tea polyphenols 0.15%, chitosan 0.03%, vitamin E 0.03%, bamboo leaf antioxidant 0.02%, fructooligosaccharide 2%, mogroside 0.0005%, stabilizer 0.12%, malic acid 0.12%, and the balance deionized water; wherein, the chitosan forms hydrogen bonds with tea polyphenols through the amino groups in its molecular structure, and adsorbs metal ions in the drink through positive charges to inhibit the oxidation of tea polyphenols and the complexation precipitation of metal ions.

[0049] Example 3: A drink containing tea polyphenols, including the following components in mass percentage: tea polyphenols 0.4%, chitosan 0.08%, vitamin E 0.07%, bamboo leaf antioxidant 0.05%, fructooligosaccharide 4%, mogroside 0.0015%, stabilizer 00.18%, malic acid 0.25%, and the balance deionized water; wherein, the chitosan forms hydrogen bonds with tea polyphenols through the amino groups in its molecular structure, and adsorbs metal ions in the drink through positive charges to inhibit the oxidation of tea polyphenols and the complexation precipitation of metal ions.

[0050] Refer to Figures 12 - 15 , experiments were conducted on the drinks obtained from the three examples of the present invention to verify the effects of the tea polyphenol drink formula containing chitosan in terms of stability, taste, and processing adaptability, including inhibiting the oxidation of tea polyphenols, the complexation precipitation of metal ions, and improving the comprehensive quality of the drink.

[0051] I. Experimental principle (I) Mechanism of action of core components Multiple stabilizing effects of chitosan: The amino group forms hydrogen bonds with tea polyphenols to stabilize their molecular structure and inhibit oxidative browning; The positive charge adsorbs negatively charged metal ions (such as Fe³⁺, Cu²⁺) in fruit juice to prevent the complex precipitation of tea polyphenols - metal ions; A surface protective film is formed to isolate oxygen and delay the oxidation reaction.

[0052] Antioxidant synergistic system: Vitamin E (liposoluble) has antioxidant activity at the oil - water interface, and bamboo leaf antioxidants (water - soluble) scavenge free radicals, forming a dual - system antioxidant network with tea polyphenols.

[0053] Stabilizer compounding effect: Gellan gum (1 part) and HPMC (1.5 parts) form a tough gel network to encapsulate unstable components and maintain uniformity after high - temperature sterilization.

[0054] Taste optimization mechanism: Fructooligosaccharides weaken the astringency of tea polyphenols, mogroside provides high - fold sweetness, and malic acid adjusts the pH to acidic (3.5 - 4.5) to balance the taste.

[0055] (II) Detection principle Stability: The color difference meter (ΔE) characterizes color changes, the turbidimeter (NTU) detects turbidity, and the centrifugal weighing method measures the precipitation amount.

[0056] Taste: The sensory evaluation method quantifies sweetness, astringency and coordination.

[0057] Rheological properties: The rheometer measures the viscosity at different shear rates to evaluate the processing fluidity.

[0058] Microbial indicators: The plate counting method is used to determine the total number of colonies, and the MPN method is used to detect coliform bacteria.

[0059] II. Experimental objects Experimental group drinks: Prepared according to the formula of Example 1, with 0.3% tea polyphenols, 0.05% chitosan, 0.05% vitamin E, 0.035% bamboo leaf antioxidants, 3% fructooligosaccharides, 0.001% mogroside, 0.15% stabilizer, and 0.18% malic acid.

[0060] Control group drinks: Traditional tea polyphenol drink formula (without chitosan, using 0.2% sodium alginate as the stabilizer).

[0061] III. Experimental steps (I) Drink preparation (experimental group) Chitosan pretreatment: Weigh 0.05 g of chitosan, add 50 mL of deionized water, stir in a water bath at 50 °C for 30 min until completely dissolved to obtain a 0.1% chitosan solution.

[0062] Preparation of basic solution: Add 0.25 g of tea polyphenols, 0.05 g of vitamin E, and 0.03 g of bamboo leaf antioxidant in sequence, and stir until dissolved; Add 3 g of fructooligosaccharide and 0.001 g of mogroside, and continuously stir for 10 min; Dropwise add 0.2 g of malic acid and adjust the pH to 4.0 (monitored in real time with a pH meter).

[0063] Compound stabilizer: Weigh 0.06 g of gellan gum and 0.09 g of HPMC, mix them and slowly add them to the basic solution, and stir at high speed (1500 rpm) for 20 min to form a uniform colloid.

[0064] Volume fixing and sterilization: Add deionized water to make the volume up to 100 g, stir evenly, then dispense into sterilized bottles, sterilize at 121 °C for 15 min, and cool to room temperature.

[0065] (II) Preparation of control group According to the traditional formula (0.25% tea polyphenols, 0.2% sodium alginate, 5% sucrose, 0.3% citric acid), the steps are the same as those of the experimental group, and the addition of chitosan is omitted.

[0066] (III) Detection items and methods Stability detection Color difference: After sterilization, after storage for 30 days and 90 days, measure L* (brightness), a* (red-green value), and b* (yellow-blue value) with a color difference meter, and calculate ΔE = √[(ΔL*)²+(Δa*)²+(Δb*)²].

[0067] Turbidity: Directly measured with a turbidimeter, unit NTU.

[0068] Precipitation amount: Take 100 mL of the beverage, centrifuge at 3000 rpm for 10 min, collect the precipitate, dry it and weigh it, unit g / L.

[0069] Taste evaluation 10 evaluators score the sweetness (0 - 5 points, 5 points being the best), astringency (0 - 5 points, 0 points being no astringency), and sourness coordination (0 - 5 points, 5 points being the most coordinated), and calculate the average score.

[0070] Rheological properties Set the shear rate of the rheometer to 10, 50, 100 s⁻¹, and measure the viscosity (mPa・s).

[0071] Microbiological detection After sterilization and storage for 90 days, take 1 mL of the drink, dilute it in gradient, inoculate it onto nutrient agar medium, and culture it at 37 °C for 48 h. Count the total number of colonies (CFU / mL); use the multiple-tube fermentation method to detect coliforms (MPN / 100 mL).

[0072] IV. Original Data Record Sheet for Experiments Stability test data (see Figure 12 ); Taste evaluation data (see Figure 13 ); Rheological property data (see Figure 14 ); Microbiological test data (see Figure 15 ).

[0073] V. Experimental Results Stability: After 90 days of storage in the experimental group, the ΔE was only 1.2, the turbidity was 6.0 NTU, and the precipitation amount was 0.2 g / L, which were significantly lower than those in the control group (ΔE = 9.5, turbidity = 35.0 NTU, precipitation = 3.5 g / L), and the stability was improved by more than 55%.

[0074] Taste: The scores of sweetness, astringency, and sourness coordination in the experimental group were 4.2, 1.0, and 4.3 respectively, all better than those in the control group (3.0, 3.5, 3.2), and the astringency was almost completely inhibited.

[0075] Rheological properties: The viscosity of the experimental group decreased significantly with the increase of shear rate, showing the characteristics of a pseudoplastic fluid and good processing fluidity; the viscosity of the control group was higher.

[0076] Microbiological indicators: After 90 days of storage in the experimental group, the total number of colonies was 45 CFU / mL, and coliforms were not detected; the total number of colonies in the control group exceeded the standard, and coliforms were positive, and the shelf life was extended by about 2 times.

[0077] VI. Conclusion Experimental data show that chitosan effectively inhibits the oxidation of tea polyphenols (the increase in color difference ΔE is reduced by 87%) and the complex precipitation of metal ions (the precipitation amount is reduced by 94%) through hydrogen bond action and electrostatic adsorption, and its function is completely different from that of traditional flocculants.

[0078] When the chitosan addition amount is 0.05%, it neither causes abnormal viscosity of the drink (rheological data shows that the viscosity is lower than that of the control group) nor produces off-flavors, proving that its dosage range is scientific and reasonable.

[0079] Through systematic testing, this experiment proves that the tea polyphenol drink formula containing chitosan is significantly superior to the traditional formula in terms of stability, taste, process adaptability, and shelf life, and has industrial promotion value.

[0080] Example 4: Refer to Figures 1 - 9 , a separation device, comprising: A separation barrel 100, an air delivery pipe 101 is installed at the bottom of the separation barrel 100, a cover plate 300 is installed at the top of the separation barrel 100, and the air delivery pipe 101 is used to deliver supercritical carbon dioxide into the separation barrel 100; A moving plate 200, installed in the separation barrel 100, a collection groove 201 is formed at the bottom of the moving plate 200, a first elastic member 203 is installed between the moving plate 200 and the cover plate 300, the first elastic member 203 provides elastic support for the moving plate 200, and the moving plate 200 is arranged such that when supercritical carbon dioxide enters the bottom of the separation barrel 100 and flows through the raw material bed layer, it carries the dissolved tea polyphenols and moves upward. As the amount of supercritical carbon dioxide continuously increases, the pressure inside the barrel rises, and the moving plate 200 is squeezed upward by the pressure. When the supercritical carbon dioxide extracts the raw materials, it also extracts the sulfides in the raw materials. The sulfides float in the supercritical carbon dioxide due to density differences and finally accumulate in the top region of the supercritical carbon dioxide, and the sulfides are in the collection groove 201. The purpose of setting the moving plate 200 is to extend the upward flow time of the supercritical carbon dioxide. Since the first elastic member 203 can provide a certain supporting force for the moving plate 200, the supporting force of the first elastic member 203 causes the moving plate 200 to slowly move upward to extend the flow time of the supercritical carbon dioxide. Only when the pressure inside the separation barrel 100 gradually becomes greater than the elastic force of the first elastic member 203, the moving plate 200 gradually moves upward, and the moving plate 200 provides time for the separation of the supercritical carbon dioxide and the sulfides; The first collection tube 400 penetrates through the cover plate 300 and the separation barrel 100 at both ends respectively. Collection holes 401 are formed on the first collection tube 400. The collection holes 401 are used to collect the supercritical fluid phase rich in target components formed after dissolving tea polyphenols. A control head 402 is installed inside the first collection tube 400. The control head 402 covers the collection holes 401. The control head 402 moves to control the opening and closing of the collection holes 401. A second elastic member 403 is installed on the control head 402. One end of the second elastic member 403 is connected to the top wall of the first collection tube 400. The second elastic member 403 is made of a stainless steel spring or can also be made of silicone rubber. A control rod 404 is installed at the top end of the control head 402. An air vent hole 301 is formed on the cover plate 300. One end of the control rod 404 extends to the outside of the first collection tube 400 and passes through the air vent hole 301 and is placed inside the separation barrel 100. A connection head 405 is installed on the control rod 404. A telescopic groove is formed on the connection head 405. The control rod 404 is connected inside the telescopic groove. The connection head 405 can move on the control rod 404. During the upward movement of the moving plate 200, it contacts the connection head 405. The moving plate 200 can drive the connection head 405 to move upward. The connection head 405 can move a certain distance on the control rod 404. When the connection head 405 moves upward, it first enters the air vent hole 301 and blocks the air vent hole 301. At this time, sulfides are collected first. During this process, the first elastic member 203 provides support for the control head 402 and the control rod 404, and the control rod 404 does not move upward until the bottom wall of the telescopic groove contacts the end of the control rod 404. The connection head 405 can drive the control rod 404 to move upward. The control rod 404 drives the control head 402 to move upward and open the collection holes 401. Then the collection holes 401 collect the supercritical fluid phase rich in target components formed after dissolving tea polyphenols; The second collection tube 500 is installed on the moving plate 200. One end of the second collection tube 500 extends into the collection groove 201. The second collection tube 500 is used to collect sulfides when the moving plate 200 moves upward to the top area of the separation barrel 100; The stirring assembly is installed on the moving plate 200 and is used to stir the raw materials.

[0081] In this embodiment, the dynamic pressure response mechanism between the separation barrel 100 and the moving plate 200: Supercritical carbon dioxide (SC-CO 2 ) is injected into the bottom of the separation barrel 100 through the gas transmission pipe 101, and the top cover plate 300 is closed to form a high-pressure environment; The moving plate 200 is horizontally placed inside the separation barrel 100. A collection groove 201 is formed at the bottom, and the top is connected to the cover plate 300 through the first elastic member 203; SC-CO 2 is injected from the bottom and carries tea polyphenols and sulfides to move upward when flowing through the raw material bed. As the SC-CO2 As the quantity increases, the pressure inside the barrel rises, and the moving plate 200 is pushed by the pressure to slowly move upward against the elastic force of the first elastic member 203; The elastic coefficient of the first elastic member 203 is set to 200 - 500 N / m (adjusted according to the volume of the separation barrel 100), so that the upward movement speed of the moving plate 200 matches the time required for the stratification of sulfides. The first elastic member 203 is made of a stainless steel spring or can also be made of silicone rubber; The sulfides float to the collection tank 201 due to their density being lower than that of SC - CO 2 and the delayed rise of the moving plate 200 ensures the full enrichment of sulfides.

[0082] Staged collection control of the first collection pipe 400 and the control head 402: First stage: When the moving plate 200 rises, it pushes the connecting head 405 into the vent hole 301 and closes it. At this time, the air pressure inside the barrel further increases, and the sulfides are locked in the collection tank 201. The control head 402 remains the collection hole 401 closed under the action of the second elastic member 403 to prevent the premature outflow of the supercritical fluid phase after dissolving tea polyphenols; Second stage: When the moving plate 200 continues to rise until the bottom wall of the telescopic groove contacts the end of the control rod 404, the connecting head 405 drives the control head 402 to move upward, and the collection hole 401 gradually opens. The opening area of the collection hole 401 has a linear relationship with the displacement of the moving plate 200, and the flow rate is dynamically adjusted through the control head 402.

[0083] The second collection pipe 500 includes: A first one - way valve 202, installed at the air inlet of the second collection pipe 500. The first one - way valve 202 is set to only allow gas to flow unidirectionally from the collection tank 201 into the second collection pipe 500; A first piston head 503, installed inside the second collection pipe 500. The first piston head 503 is driven by a control mechanism to adsorb the sulfides in the collection tank 201. When the first piston head 503 moves inside the second collection pipe 500, the second collection pipe 500 can adsorb and collect the sulfides in the collection tank 201; A valve nozzle 502, installed on the second collection pipe 500. After opening the switch of the valve nozzle 502, the sulfides collected by the second collection pipe 500 can be discharged; A control mechanism, installed on the second collection pipe 500. The control mechanism is connected to the first piston head 503 and is used to control the movement of the first piston head 503 inside the second collection pipe 500.

[0084] Sulfide adsorption mechanism of the second collection pipe 500 and the control mechanism: After the vent hole 301 is closed, the air pressure between the moving plate 200 and the cover plate 300 increases, pushing the second piston head 505 to move along the connecting pipe 501, driving the first piston head 503 to suck sulfide.

[0085] Air pressure drive parameters: working pressure 5 - 10 MPa, piston stroke 50 - 100 mm.

[0086] The control mechanism includes a connecting pipe 501, a second piston head 505 and a moving rod 504. The connecting pipe 501 is arranged in the second collecting pipe 500, one end of the connecting pipe 501 extends to the outside of the second collecting pipe 500, the second piston head 505 is installed in the connecting pipe 501, one end of the moving rod 504 is connected to the second piston head 505, and the other end of the moving rod 504 is connected to the first piston head 503. After the connector 405 enters the vent hole 301, the gas between the moving plate 200 and the cover plate 300 cannot be discharged from the vent hole 301. When the moving plate 200 continues to move upward, it will squeeze the gas between the moving plate 200 and the cover plate 300, increasing the air pressure between the moving plate 200 and the cover plate 300 to push the second piston head 505 to move in the connecting pipe 501. The second piston head 505 drives the moving rod 504 and the first piston head 503 to move, and the first piston head 503 drives the second collecting pipe 500 to adsorb and collect the sulfide in the collecting groove 201; The stirring assembly includes: a connecting sleeve 601, which is movably sleeved on the first collecting pipe 400 and rotatably connected to the moving plate 200; a stirring rod 600, which is installed on the connecting sleeve 601; a moving groove 603, which is opened on the outer surface of the first collecting pipe 400, and the moving groove 603 is spiral. The stirring rod 600 cooperates with the moving groove 603 through a moving block 602, so that when the moving plate 200 rises, it drives the stirring rod 600 to rotate around the first collecting pipe 400 and stir the raw materials. During the upward movement of the moving plate 200, it drives the connecting sleeve 601 and the stirring rod 600 to move upward. The moving block 602 moves along the moving groove 603, enabling the stirring rod 600 to drive the connecting sleeve 601 to rotate around the first collecting pipe 400. The stirring rod 600 can play a role in stirring the raw materials, enabling supercritical carbon dioxide to fully contact the raw materials.

[0087] The opening area of the collecting hole 401 has a linear relationship with the displacement of the moving plate 200 and is dynamically adjusted by the control head 402.

[0088] Example Five: The difference between this example and Example Four is as follows, referring to Figure 10 , the control mechanism includes a first power source 506, which is installed on the second collecting pipe 500. The power shaft of the first power source 506 is connected to the first piston head 503 for controlling the movement of the first piston head 503. The first power source 506 uses a stepper motor or a servo motor can also be used.

[0089] Reference Figure 11 , the stirring assembly includes a stirring rod 600 and a second power source 604. The stirring rod 600 is installed below the moving plate 200, and the second power source 604 is installed on the moving plate 200. The output shaft of the second power source 604 is connected to the stirring rod 600. The second power source 604 drives the stirring rod 600 to rotate. The second power source 604 uses a stepper motor or a servo motor can also be used.

[0090] Working process of the tea polyphenol-containing beverage separation device 1. Initial stage: Device startup and raw material loading Step 1: Raw material filling Load the raw material containing tea polyphenols (such as tea powder) into the bottom of the separation barrel 100, and the filling height is 60%-70% of the volume of the separation barrel 100; Close the cover plate 300 to ensure airtightness.

[0091] Step 2: Supercritical carbon dioxide injection Inject supercritical carbon dioxide (SC-CO 2 ) into the separation barrel 100 through the gas transmission pipe 101. The initial pressure is set to 5 MPa and the temperature is 35 °C; SC-CO 2 The flow rate is controlled at 10 L / min and the injection continues until the pressure in the barrel rises to 8 MPa.

[0092] 2. Pressure accumulation and sulfide enrichment stage Step 3: Dynamic response of the moving plate 200 SC-CO 2 flows through the raw material bed, dissolves tea polyphenols and carries sulfides upward; The pressure in the barrel gradually increases with the increase of the amount of SC-CO 2 , and the moving plate 200 is pushed by the pressure to slowly move upward against the elastic force of the first elastic member 203; Sulfides float to the collection tank 201 at the bottom of the moving plate 200 due to density differences (SC-CO 2 density ≈ 0.7 g / cm³, sulfide density ≈ 0.1 g / cm³).

[0093] Step 4: Sulfide locking During the upward movement of the moving plate 200, the connecting head 405 enters the vent hole 301 of the cover plate 300 and closes it; At this time, a sealed high-pressure chamber is formed in the separation barrel 100, and the sulfides are locked in the collection tank 201.

[0094] 3. Sulfide collection stage Step 5: The second collection pipe 500 starts adsorption Pneumatic drive mode (Example 4): The air pressure between the moving plate 200 and the cover plate 300 is increased to 10 MPa, pushing the second piston head 505 to move along the connecting pipe 501; The second piston head 505 drives the first piston head 503 to suck sulfide through the moving rod 504, and the adsorption stroke is 80 mm.

[0095] Power source drive mode (Example 5): Start the stepper motor to drive the first piston head 503 to move at a speed of 10 mm / s to complete the sulfide adsorption.

[0096] Step 6: Sulfide discharge Open the valve nozzle 502 of the second collection pipe 500 and discharge the sulfide to the external treatment device through the pressure relief valve.

[0097] 4. Tea polyphenol collection stage Step 7: Dynamically open the first collection hole 401 When the moving plate 200 continues to rise until the bottom wall of the telescopic groove contacts the end of the control rod 404, the connector 405 drives the control head 402 to move upward; The control head 402 gradually opens the collection hole 401, and the opening area has a linear relationship with the displacement; The tea polyphenol phase (containing SC-CO 2 ) enters the first collection pipe 400 through the collection hole 401, and the flow rate is dynamically adjusted by the position of the control head 402.

[0098] Step 8: Separation and recovery of the tea polyphenol phase The SC-CO 2 fluid rich in tea polyphenols is transported to the decompression separation kettle through the first collection pipe 400, and the tea polyphenols are precipitated by reducing the pressure (5 MPa → 0.1 MPa); The recovery rate of tea polyphenols ≥ 96% (detected by HPLC).

[0099] 5. Dynamic mixing of the stirring assembly Step 9: Linkage operation of the stirring rod 600 When the moving plate 200 rises, the connecting sleeve 601 drives the stirring rod 600 to rotate through the spiral moving groove 603; The stirring rod 600 stirs the raw materials to increase the contact area between the raw materials and SC-CO 2 .

[0100] In summary, compared with the prior art, the following beneficial effects are achieved: The molecular structure of tea polyphenols is stabilized through hydrogen bonding, effectively delaying oxidation; at the same time, the positive charge characteristics are used to adsorb metal ions in the beverage to prevent the metal ions from complexing with tea polyphenols to form precipitation; vitamin E and bamboo leaf antioxidants are compounded to form an antioxidant network covering both oil and water phases, significantly enhancing the free radical scavenging ability of the beverage.

[0101] Oligofructose provides a soft sweetness and weakens the astringency. Mongoside accurately adjusts the sweetness to avoid the health risks of high sugar or artificial sweeteners, while improving the palatability of the beverage. Oligofructose promotes intestinal health, and malic acid coordinates the flavor, forming a beverage system that is both functional and natural in flavor.

[0102] The movable plate 200 rises slowly through the elastic support of the first elastic member 203, prolonging the flow time of the supercritical carbon dioxide in the separation barrel 100, ensuring that the sulfide fully floats up and is enriched in the collection tank 201 due to the density difference. When the movable plate 200 rises, the vent hole 301 is closed to form a closed high-pressure environment, forcing the sulfide to remain in the collection tank 201. The opening area of ​​the collection hole 401 is dynamically adjusted by the control head 402 to achieve directional and efficient recovery of the tea polyphenol phase.

[0103] The second collecting tube 500 rises synchronously with the moving plate 200 to the top of the separation barrel 100. The one-way valve at its air inlet ensures the one-way inflow of sulfide. When the moving plate 200 closes the vent 301, the increased air pressure in the barrel drives the piston head to adsorb the sulfide and discharge it directly through the second collecting tube 500, thereby avoiding the deposition of thiocarbonate in valves or pipes.

[0104] When the movable plate 200 rises, the spiral groove drives the stirring rod 600 to rotate, forcibly crushing the raw materials and enhancing the contact efficiency between the supercritical carbon dioxide and the materials, thereby improving the extraction rate of tea polyphenols. Sulfide separation and tea polyphenols collection are completed in stages through the same device, reducing the efficiency loss caused by switching of multiple equipment in traditional processes.

[0105] Thus, although the invention has been described herein with reference to specific embodiments thereof, freedom of modification, various changes and substitutions are also within the foregoing disclosure, and it should be understood that in some cases, some features of the invention will be employed without the corresponding use of other features without departing from the scope and spirit of the proposed invention. Thus, many modifications may be made to adapt a particular environment or material to the essential scope and spirit of the invention. The invention is not intended to be limited to the specific terms used in the claims below and / or the specific embodiments disclosed as the best mode contemplated for carrying out the invention, but the invention will include any and all embodiments and equivalents falling within the scope of the appended claims. Thus, the scope of the invention will be determined solely by the appended claims.

Claims

1. A separation device, characterized in that: include: A separation barrel (100), wherein a gas delivery pipe (101) is installed at the bottom of the separation barrel (100) and a cover plate (300) is installed at the top, wherein the gas delivery pipe (101) is used to deliver supercritical carbon dioxide into the separation barrel (100); A movable plate (200) is installed in the separation barrel (100); a collecting groove (201) is provided at the bottom of the movable plate (200); a first elastic member (203) is installed between the movable plate (200) and the cover plate (300); the movable plate (200) is configured to move upward under the pressure of the supercritical carbon dioxide to extend the stratification time of the supercritical carbon dioxide and the sulfide; A first collecting tube (400), with two ends respectively penetrating the cover plate (300) and the separation barrel (100), and a collecting hole (401) is provided on the first collecting tube (400) for collecting the supercritical fluid phase after the tea polyphenols are dissolved; A second collecting pipe (500) is mounted on the moving plate (200), one end of which extends into the collecting tank (201), and is used to collect sulfide when the moving plate (200) moves to the top area of ​​the separation barrel (100); The first piston head (503) is installed in the second collecting tube (500), and the first piston head (503) is driven by the control mechanism to adsorb the sulfide in the collecting tank (201).

2. The separation device according to claim 1, characterized in that: The first collecting tube (400) comprises: A control head (402) is installed in the first collecting tube (400), and the control head (402) covers the collecting hole (401); A second elastic member (403), one end of which is mounted on the control head (402), and the other end of which is mounted on the top wall of the first collecting tube (400); A control rod (404) is mounted on the top of the control head (402); a vent hole (301) is provided on the cover plate (300); one end of the control rod (404) extends to the outside of the first collecting pipe (400) and passes through the vent hole (301) to be placed in the separation barrel (100); The connector (405) is mounted on the control rod (404). The connector (405) is provided with a telescopic slot. The control rod (404) is connected to the telescopic slot. When the movable plate (200) moves upward, the connector (405) is first pushed into the vent (301) and blocks the vent (301) until the bottom wall of the telescopic slot contacts the end of the control rod (404). The connector (405) drives the control rod (404) to move upward, and the control head (402) opens the collection hole (401) to collect the supercritical fluid phase rich in tea polyphenols.

3. The separation device according to claim 2, characterized in that: The control mechanism comprises: A connecting pipe (501) is disposed in the second collecting pipe (500) and one end of which extends outside the connecting pipe (501); The second piston head (505) is installed in the connecting pipe (501); A moving rod (504), one end of which is connected to the second piston head (505), and the other end of which is connected to the first piston head (503); When the connecting head (405) blocks the vent hole (301), the air pressure between the movable plate (200) and the cover plate (300) increases, pushing the second piston head (505) to move in the connecting tube (501), and driving the first piston head (503) to move in the second collecting tube (500) through the moving rod (504) to adsorb sulfide.

4. The separation device according to claim 1, characterized in that: The control mechanism comprises a first power source (506) installed on the second collecting tube (500), and a power shaft of the first power source (506) is connected to the first piston head (503) for controlling the movement of the first piston head (503) in the second collecting tube (500).

5. The separation device according to claim 1, characterized in that: The gas inlet of the second collecting pipe (500) is installed with a first one-way valve (202), and the first one-way valve (202) is configured to only allow gas to flow from the collecting tank (201) into the second collecting pipe (500) in one direction.

6. The separation device according to claim 1, characterized in that: The second collecting pipe (500) is provided with a valve (502) for discharging the collected sulfide after opening.

7. The separation device according to claim 1, characterized in that: It also includes a stirring assembly, which is installed on the moving plate (200) and is used to stir the raw materials.

8. The separation device according to claim 7, characterized in that The stirring assembly comprises: A connecting sleeve (601), the connecting sleeve (601) is movably sleeved on the first collecting tube (400) and is rotatably connected to the movable plate (200); A stirring rod (600) is mounted on the connecting sleeve (601); The movable groove (603) is formed on the outer surface of the first collecting tube (400), and is spiral-shaped. The stirring rod (600) cooperates with the movable groove (603) through the movable block (602), so that when the movable plate (200) rises, the stirring rod (600) is driven to rotate around the first collecting tube (400) and stir the raw materials.

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