Olive essence preparation and mixing device and method
Through the mixing method of mesoporous silica-encapsulated olive polyphenols and phospholipid bilayer liposomes encapsulated ceramide NP, combined with the double buffering system of disodium hydrogen phosphate and citric acid, the double embedding and laminar flow mixing technology is used to solve the problem of destruction of active structure during the mixing of multi-active ingredients in the essence, and the multi-effect integrated oil olive essence is achieved, with antioxidant, moisturizing and acne removal effects.
Patent Information
- Application Number
- CN202510265362.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-07
- Publication Date
- 2025-04-04
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
The existing essence products have single effects. During the mixing process, the active structure of multi-active ingredients is damaged due to microenvironment adaptation conflicts and the mixing process, and the mixing process cannot effectively modulate and mix, resulting in insufficient activity and synergistic effects not being realized.
The mixing method of mesoporous silica-encapsulated olive polyphenols and phospholipid bilayer liposomes encapsulated ceramide NP is adopted, combined with the double buffering system of disodium hydrogen phosphate and citric acid. The pH value and Reynolds number are controlled through double embedding and laminar flow mixing technology to ensure the efficient coexistence of salicylic acid and ceramide NP.
It has achieved a multi-effect integrated oil and olive essence, covering the three major needs of antioxidant, moisturizing and acne removal, effectively removing red blood, inhibiting acne regeneration, fading acne marks, repairing damaged skin, and restoring the natural and healthy skin state.
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Figure CN119745707A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of essence preparation and mixing, and in particular to an olive essence preparation and mixing device and method. Background Art
[0002] As a highly concentrated skin care preparation, the core value of essence lies in achieving targeted skin care effects through the synergistic effect of rare active ingredients. Olive (Olea europaea) leaf extract is rich in polyphenols such as oleuropein and hydroxytyrosol, and has shown significant advantages in anti-oxidation (ROS scavenging ability reaches IC50 8.3μM), anti-inflammatory (inhibiting TNF-α secretion by >65%) and barrier repair, and has now become the preferred ingredient for high-end functional essences.
[0003] The current essences on the market generally have the defect of single efficacy: moisturizing products rely on ceramide complexes, acne-removing formulas focus on salicylic acid controlled-release systems, and antioxidant products focus on vitamin C derivatives.
[0004] This single-effect orientation stems from several problems with the coexistence of multiple active ingredients, such as microenvironment adaptation conflicts and mixing process destruction of active structures. As a result, multiple active ingredients with different functions cannot be modulated and mixed together, resulting in no synergistic effect and increased skin care effects. It may even lead to insufficient activity and inability to maintain the original effect.
[0005] Therefore, it is necessary to provide an olive essence liquid modulation and mixing device and method to solve the above-mentioned technical problems. Summary of the invention
[0006] The invention overcomes the shortcomings of the prior art and provides an olive essence liquid preparation and mixing device and method.
[0007] To achieve the above object, the technical solution adopted by the present invention is: a method for preparing and mixing olive essence, comprising the following steps: S1. Mixing olive polyphenols encapsulated by mesoporous silica with ceramide NPs encapsulated by phospholipid bilayer liposomes, adding disodium hydrogen phosphate buffer to adjust the pH value to 5.0-5.8, stirring at a low speed and then homogenizing at a high speed, adding phytosterols simultaneously, and heating to 50-60° C. for 10-20 min, and cooling to obtain component A; S2, mixing the salicylic acid-HPβCD inclusion complex embedded in mesoporous silica with PCA zinc in glycerol, adjusting the pH value to 2.7-3.5 by adding citric acid buffer, and stirring at a low speed for 20-30 minutes to obtain component B; S3, preliminarily mix component B and component A, add triethanolamine simultaneously, keep the mixing temperature at 50-53°C, and control the pH value between 4.8 and 5.0; After the initial mixing is completed, polyglycerol-10 laurate is added and stirred continuously at 54-58°C for 10-20 minutes to form a mixed system; S4, pre-gelling Carbopol Ultrez 21 and propylene glycol, and injecting them into the mixed system through a static mixer to generate component C; S5. After adding ethylhexylglycerol and tocopherol acetate to component C, nitrogen bubbling deoxygenation, vacuum degassing and filtration are performed in sequence to obtain the olive essence.
[0008] In a preferred embodiment of the present invention, in S3, the Reynolds number of the preliminary mixing process is controlled within the range of 1000 to 2000.
[0009] In a preferred embodiment of the present invention, in S3, when pumping component B into component A, the diameter of the component B channel pipe used is 4-7 mm, and the flow rate of component B is 0.4-0.8 L / min.
[0010] In a preferred embodiment of the present invention, in S1, the low-speed stirring rate is 100-300 rpm, and the time is 5-15 min; The high-speed homogenization rate is 7000-9000rpm, and D90 after homogenization is less than 150nm.
[0011] In a preferred embodiment of the present invention, in said S2, the method for preparing the mesoporous silica secondary embedding salicylic acid-HPβCD inclusion complex comprises: S21, including salicylic acid and hydroxypropyl-β-cyclodextrin in a molar ratio of 1:2 to 3; S22. Using mesoporous silica to perform secondary encapsulation of the salicylic acid-HPβCD inclusion complex prepared in S21.
[0012] In a preferred embodiment of the present invention, in S1, the mass ratio of the mesoporous silica-encapsulated olive polyphenol and the phospholipid bilayer liposome-encapsulated ceramide NP when mixed is 0.5-2:9.
[0013] In a preferred embodiment of the present invention, in said S4, the control parameters of the static mixer are: linear velocity of 0.5-1 m / s, and shear rate of 800-1200 s-1.
[0014] In a preferred embodiment of the present invention, in S3, triethanolamine is dynamically added through an online sensor to ensure that the pH value of the preliminary mixed system is stabilized between 4.8 and 5.0.
[0015] In a preferred embodiment of the present invention, the addition amount of PCA zinc in S2 is 5%.
[0016] In a preferred embodiment of the present invention, in the component B, the concentration of free salicylic acid is ≤0.1%.
[0017] In a preferred embodiment of the present invention, the viscosity of component C is 4000-5000 CPS.
[0018] An olive essence preparation and mixing device, used in any of the olive essence preparation and mixing methods described above, comprising: The mixing mechanism comprises a dynamic mixing tank and a three-channel dosing assembly arranged on the dynamic mixing tank; the dynamic mixing tank is used for mixing component A and component B; Gel mechanism for pre-gelling of Carbopol Ultrez 21 with propylene glycol; Static mixer, used to inject pre-gel into the main mixing system; An injection pump is connected to the static mixer to pump the main mixing system and the pre-gel into the static mixer respectively; And post-processing components, including nitrogen bubbling tower, vacuum degassing tank and filter element.
[0019] In a preferred embodiment of the present invention, the three-channel dosing assembly comprises: A component B channel configured as a plurality of orifices surrounding the side wall of the dynamic mixing tank; A pH adjustment channel is arranged at the upper part of the dynamic mixing tank; The additive channel is arranged at the upper part of the dynamic mixing tank.
[0020] The present invention solves the defects existing in the background technology and has the following beneficial effects: (1) The present invention provides a method for preparing and mixing olive essence, which uses double encapsulation to isolate salicylic acid and ceramide NP, and combines a citric acid-disodium hydrogen phosphate double buffer system to control pH in a partitioned manner, so as to effectively prepare and mix olive extract, ceramide and salicylic acid, thereby ensuring the activity of salicylic acid and avoiding the destruction of ceramide structure, thereby preparing a multi-effect olive essence that covers the three major needs of anti-oxidation, moisturizing and acne removal, can effectively remove red blood streaks, help inhibit acne regeneration, fade acne marks, repair damaged skin, and restore the skin to its natural healthy state.
[0021] (2) The present invention uses phospholipid bilayer liposomes to encapsulate ceramide NP. Ceramide NP acts as a moisturizing core to supplement stratum corneum lipids and repair the barrier, while liposomes enhance transdermal efficiency and maintain the stability of the liquid crystal structure, that is, maintain pH 5.0 to 5.8 to adapt to the physiological environment. Disodium hydrogen phosphate buffer is used to maintain the stable pH of ceramide NP liposomes within the range of 5.0 to 5.8, prevent the collapse of the lamellar structure, enhance the tolerance of the ceramide NP liquid crystal structure to low pH, and reduce the risk of system stratification after mixing.
[0022] (3) The present invention uses precise inclusion and secondary embedding technology to ensure the high acne-removing activity of salicylic acid while minimizing its effect on the stability of ceramide NP, providing core technical support for the multi-effect all-in-one essence. Specifically, secondary embedding of mesoporous silica can achieve pH-responsive release of salicylic acid, that is, the pores open when pH is less than 3.5, targeting the acidic microenvironment of acne lesions.
[0023] (4) The present invention controls the Reynolds number of the fluid in the preliminary mixing process, that is, based on the fluid viscosity, adjusts the pumping rate, pipe diameter and stirring speed of component B to control the Reynolds number within the range of 1000 to 2000, thereby ensuring that components B and A are initially mixed in a laminar flow mode, which can reduce the mechanical shear force on sensitive components when component B is pumped in, and control the mechanical impact energy in the preliminary mixing process below the critical rupture threshold of the liposome of component B, thereby improving the encapsulation rate of ceramide NP in the mixed system, and the lamellar liquid crystal structure can remain intact.
[0024] (5) The present invention realizes "microenvironment customization" of the active ingredients on a molecular scale by double encapsulation and isolation of salicylic acid and by combining a dual buffer pair of disodium hydrogen phosphate (component A) and citric acid (component B), thereby achieving efficient coexistence of salicylic acid and ceramide, that is, salicylic acid maintains its activity at a low pH (2.7-3.5), ceramide NP maintains its structure at a neutral to acidic temperature (5.0-5.8), and the pH of the system after mixing is stabilized at 4.8-5.0, thereby avoiding conflicts between the components. BRIEF DESCRIPTION OF THE DRAWINGS
[0025] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art are briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present invention. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative work. Figure 1 2. It is a diagram of a method for preparing and mixing olive essence according to a preferred embodiment of the present invention; Figure 2It is a diagram of the preparation method of mesoporous silica secondary embedding salicylic acid-HPβCD inclusion complex according to a preferred embodiment of the present invention; Figure 3 is a schematic diagram of the structure of a mixing mechanism of a preferred embodiment of the present invention; In the figure: 100, dynamic mixing tank; 200, B component channel; 300, pH adjustment channel; 400, additive channel. DETAILED DESCRIPTION
[0026] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0027] In the following description, many specific details are set forth to facilitate a full understanding of the present invention, but the present invention may also be implemented in other ways different from those described herein. Therefore, the protection scope of the present invention is not limited to the specific embodiments disclosed below.
[0028] In the description of the present application, it should be understood that the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", etc., indicating orientations or positional relationships, are based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the scope of protection of the present application.
[0029] In the description of this application, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, and it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in this application can be understood by specific circumstances.
[0030] like Figure 1 As shown, the present invention provides a method for preparing and mixing olive essence, comprising the following steps: S1. Mix mesoporous silica-encapsulated olive polyphenol (drug loading ≥ 15%) and phospholipid bilayer liposome-encapsulated ceramide NP (liposome particle size D50 = 80 ± 10 nm) at a mass ratio of 0.5 to 2:9, add disodium hydrogen phosphate buffer to control the pH of the mixture at 5.0 to 5.8, stir at a low speed and then homogenize at a high speed, simultaneously add 0.2% phytosterol, raise the temperature to 50 to 60°C and maintain for 10 to 20 min, and then cool to 35-45°C to obtain component A for standby use.
[0031] S2. Mix the mesoporous silica-embedded salicylic acid-HPβCD inclusion complex with 5% PCA zinc in glycerol, add citric acid buffer to control the pH at 2.7-3.5, stir at a low speed for 20-30 minutes at a stirring rate of 100-200 rpm to obtain component B, in which the concentration of free salicylic acid is ≤0.1%.
[0032] S3. Preliminarily mix component B and component A, and simultaneously add 0.5% triethanolamine to neutralize the free acid, maintain the mixing temperature at 50-53°C, and control the pH value between 4.8 and 5.0; after the preliminary mixing is completed, add 0.1% polyglycerol-10 laurate, maintain the temperature at 54-58°C and stir for 10-20 minutes to obtain a mixed system.
[0033] S4. Pre-gel 0.25% Carbopol Ultrez 21 and propylene glycol to a swelling ratio of ≥ 95%, and inject into the mixing system through a static mixer to obtain component C, which has a viscosity of 4000-5000 CPS.
[0034] S5. After adding 0.5% ethylhexylglycerol and 0.1% tocopherol acetate to component C, nitrogen bubbling deoxygenation, vacuum degassing and filtration are performed in sequence to obtain the olive essence.
[0035] The invention provides a method for preparing and mixing an olive essence, which uses double encapsulation to isolate salicylic acid and ceramide NP, combines a citric acid-disodium hydrogen phosphate double buffer system to control pH in a partitioned manner, and effectively prepares and mixes olive extract, ceramide and salicylic acid, thereby ensuring the activity of salicylic acid and avoiding structural damage to ceramide, and preparing a multi-effect olive essence, which covers the three major needs of anti-oxidation, moisturizing and acne removal, can effectively remove red blood streaks, helps inhibit acne regeneration, fades acne marks, repairs damaged skin, and restores the skin to a natural healthy state.
[0036] The following is a detailed supplementary explanation of the above steps one by one.
[0037] Step S1, preparation of component A.
[0038] S11. Preparation of mesoporous silica-encapsulated olive polyphenols, specifically comprising: 1) Raw material pretreatment: Olive leaves (active ingredient oleuropein ≥ 10%) picked from December to February of the following year were selected for supercritical CO2 extraction to obtain a polyphenol crude extract with a purity of ≥ 80%. 2 / g of mesoporous silica and dried in a dryer at 120°C for 2h to remove moisture before use.
[0039] 2) Drug delivery: 2.1) The crude olive polyphenol extract was mixed with mesoporous silica in a mass ratio of 1:2, anhydrous ethanol was added, the solid-liquid ratio was controlled within the range of 1:10, and the mixture was stirred at a constant temperature of 40°C for 2 h.
[0040] 2.2) The mixture of step 2.1 was centrifuged at 4000 rpm for 15 min to remove unadsorbed free polyphenols, and the precipitate was washed three times with deionized water.
[0041] 2.3) The washed precipitate was freeze-dried at -50°C for 24 h to obtain drug-loaded particles. The oleuropein content was detected by HPLC to control the drug loading to ≥15%.
[0042] Through the above steps, olive polyphenols are encapsulated by mesoporous silica. Olive polyphenols provide antioxidant function, that is, scavenging free radicals and inhibiting lipid peroxidation, while mesoporous silica protects olive polyphenols from oxidative degradation and controls the sustained release to improve tolerance to acidic environments.
[0043] S12, preparation of phospholipid bilayer liposomes encapsulating ceramide NPs, specifically comprising: 3) Raw material pretreatment: Hydrogenated soybean lecithin (HSPC) and cholesterol were mixed in a mass ratio of 7:3 as the main lipid. Ceramide NP with a purity of ≥95% was selected, and the total mass ratio of ceramide NP to lipid was 1:5.
[0044] 4) Lipid film formation: 4.1) Dissolve hydrogenated soybean lecithin, cholesterol, and ceramide NP in chloroform-methanol (2:1, v / v) to a total concentration of 10 mg / mL.
[0045] 4.2) The solvent prepared in 4.1 was evaporated on a rotary evaporator at 40°C, 100 rpm, and -0.08 MPa vacuum to remove the organic solvent and form a uniform lipid film on the inner wall of the flask.
[0046] 5) Hydration and homogenization: 5.1) Prepare 0.1 M sodium phosphate buffer, pH 5.5, containing 0.1% disodium EDTA, i.e., chelated metal ions.
[0047] 5.2) Add 10 volumes of disodium hydrogen phosphate buffer according to the mass of lipid film and shake in a water bath at 55°C for 30 min to form a multilamellar liposome suspension.
[0048] 5.3) The multilayer liposome suspension was passed through a high-pressure homogenizer for 3 cycles at 1000 bar to obtain phospholipid bilayer liposomes encapsulating ceramide NPs with a particle size of D50 = 80 ± 10 nm and a PDI < 0.2.
[0049] Through the above steps, phospholipid bilayer liposomes are used to encapsulate ceramide NP. Ceramide NP serves as a moisturizing core, replenishes stratum corneum lipids, and repairs the barrier, while liposomes enhance transdermal efficiency and maintain the stability of the liquid crystal structure, that is, maintain an adaptive physiological environment of pH 5.0 to 5.8.
[0050] It is worth mentioning that the disodium hydrogen phosphate buffer is used to maintain the stable pH of the ceramide NP liposomes in the range of 5.0 to 5.8, prevent the collapse of the lamellar structure, enhance the tolerance of the ceramide NP liquid crystal structure to low pH, and reduce the risk of stratification of the system after mixing.
[0051] S13. A method for preparing component A, comprising: 6) Premix the mesoporous silica-encapsulated olive polyphenols and the phospholipid bilayer liposome-encapsulated ceramide NPs at a mass ratio of 0.5 to 2:9, add deionized water to a total solid content of 5%, and stir at a low speed of 100 to 300 rpm for 5 to 15 minutes to ensure that the two substances are evenly dispersed.
[0052] 7) The uniformly dispersed mixture is homogenized at high speed at a speed of 7000-9000 rpm for 5-10 min. The homogenization process is monitored to ensure that D90 is less than 150 nm and Zeta potential is -35 mV to avoid particle aggregation.
[0053] 8) After the mixture is homogenized, 0.2% phytosterol is added immediately, and the temperature is raised to 50-60°C and maintained for 10-20 min. At the same time, a slow stirring of 100 rpm is performed to promote the insertion of sterol into the lipid bilayer. Finally, the temperature is gradually reduced to 35-45°C to obtain component A for standby use. The cooling rate is controlled at 2°C / min to avoid sudden changes in the liposome structure.
[0054] Through the above steps, through material selection, precise control of process parameters and structural enhancement technology, the excellent performance of component A in anti-oxidation, moisturizing and stability is ensured, providing an ideal base for subsequent mixing.
[0055] It is worth mentioning that mesoporous silica encapsulated olive polyphenols and ceramide NPs synergistically strengthen the skin barrier and reduce barrier damage caused by oxidative stress. Phospholipid bilayer liposomes encapsulate ceramide NPs and phytosterols to form a mixed liquid crystal phase, which prolongs the moisturizing effect. In addition, phytosterols improve the tolerance of the ceramide NP liquid crystal structure to pH 3.0-5.8.
[0056] Step S2: preparation of component B.
[0057] like Figure 2 As shown, the preparation method of mesoporous silica secondary embedding salicylic acid-HPβCD inclusion complex specifically comprises the following steps: S21, including salicylic acid and hydroxypropyl-β-cyclodextrin in a molar ratio of 1:2-3, specifically comprising: raw material: Salicylic acid: purity ≥99%, particle size D90<50μm; Hydroxypropyl-β-cyclodextrin (HPβCD): degree of substitution 0.6~0.9, moisture ≤5%.
[0058] 1) Dissolve hydroxypropyl-β-cyclodextrin in 40% ethanol aqueous solution with a solid-liquid ratio of 1:15, and stir in a water bath at 50°C until completely dissolved.
[0059] 2) Slowly add salicylic acid powder to the solution, maintain the temperature in the range of 48-52°C, and slowly stir for 6 hours in a dark environment, with the rotation speed preferably at 300 rpm.
[0060] 3) After stirring, remove unencapsulated crystals through a 0.45 μm nylon filter membrane, and use a dialysis bag with a molecular weight cutoff of 1000 Da to dialyze with pure water for 24 hours, changing the water every 4 hours to remove free drugs and solvents.
[0061] 4) After dialysis is completed, freeze-drying is performed for 24 hours at a temperature of -50°C to obtain a white powder inclusion complex.
[0062] S22, using mesoporous silica to perform secondary embedding of the salicylic acid-HPβCD inclusion complex prepared in S21, specifically comprising: raw material: Mesoporous silica: pore size 5nm, specific surface area ≥800m² / g, activated at 150℃ for 2h before use.
[0063] 5) The salicylic acid-HPβCD inclusion complex powder was mixed with mesoporous silica in a mass ratio of 1:1, anhydrous ethanol was added, the solid-liquid ratio was 1:10, and ultrasonic-assisted adsorption was performed at 40°C for 12 h. The ultrasonic parameters were controlled at 40 kHz and 200 W.
[0064] 6) After adsorption, centrifuge at 5000 rpm for 20 min, and wash the precipitate three times with deionized water to remove physically adsorbed free drugs.
[0065] 7) The precipitate was vacuum dried for 24 hours at 40°C to obtain the mesoporous silica secondary encapsulated salicylic acid-HPβCD inclusion complex.
[0066] Further, the above mesoporous silica is used to secondary embed the salicylic acid-HPβCD inclusion complex and mixed with PCA zinc to prepare component B, which specifically includes the following steps: raw material: The mesoporous silica secondary encapsulation salicylic acid-HPβCD inclusion complex was passed through a 200-mesh sieve to ensure that the particle size D90 was <50 μm; PCA zinc: purity ≥98%, particle size D50<20μm; Glycerin: pharmaceutical grade, moisture ≤ 0.5%.
[0067] 8) Premix 5% PCA zinc and embedded particles in glycerol at a mass ratio of 1:1, and stir at low speed for 10 min at 40°C and 150 rpm.
[0068] 9) After premixing, add 0.1M, pH 2.8 citric acid buffer, dynamically adjust to pH 2.7-3.5, and stir at a low speed for 25 minutes with the speed controlled at 200 rpm to ensure the ion balance of the system and uniform particle dispersion.
[0069] It is worth noting that the free salicylic acid concentration in component B is ≤0.1%, based on HPLC detection. If the free concentration is >0.1%, hydroxypropyl-β-cyclodextrin is added in a gradient of 0.5% and stirred again for 10 minutes.
[0070] The above steps, through precise inclusion and secondary embedding technology, ensure the high acne-removing activity of salicylic acid while minimizing its impact on the stability of ceramide NP, providing core technical support for the multi-effect all-in-one essence. Specifically, secondary embedding of mesoporous silica can achieve pH-responsive release of salicylic acid, that is, the pores open when pH is less than 3.5, targeting the acidic microenvironment of acne lesions.
[0071] Step S3: Component B is mixed with component A.
[0072] Component A is first placed in a dynamic mixing tank 100, equipped with an anchor stirrer with a diameter / pot diameter ratio of 0.6, and the speed is set to 30-60 rpm. A peristaltic pump is used to pump component B into component A through component B channel 200 for preliminary mixing, and the Reynolds number of the preliminary mixing process is controlled within the range of 1000-2000.
[0073] Importantly, the diameter of the B component channel 200 used in the preliminary mixing process is 4 to 7 mm, and the flow rate of the B component is controlled to be 0.4 to 0.8 L / min. In addition, the B component channel 200 is arranged in the dynamic mixing tank 100, and the B component channel 200 is divided into a plurality of pipe openings, which are distributed on the side wall of the dynamic mixing tank 100 in a circular array, and the direction of the pipe openings is consistent with the rotation direction of the agitator in the dynamic mixing tank 100.
[0074] Furthermore, the dynamic mixing tank 100 is specifically a cylindrical flat-bottom stirring tank.
[0075] The Reynolds number is a dimensionless parameter used to evaluate the state of fluid flow and distinguish between laminar flow (low Reynolds number) and turbulent flow (high Reynolds number). In this process step, the Reynolds number during the initial mixing process is precisely controlled to ensure that component B and component A are mixed in a laminar flow mode. Specific measures include adjusting the pumping rate of component B, the pipe diameter, and the speed of the agitator according to the fluid viscosity to control the Reynolds number within the range of 1000 to 2000.
[0076] This precise control not only reduces the mechanical shear force on sensitive ingredients when pumping in component B, but also ensures that the mechanical impact energy during the initial mixing process remains below the critical rupture threshold of the liposome. This helps to improve the encapsulation efficiency of ceramide NPs in the mixed system and maintain the integrity of its lamellar liquid crystal structure. Ultimately, this method achieves efficient homogenization while protecting the active ingredients.
[0077] The specific mixing process includes: 1) Component A is preheated to 50°C and component B is preheated to 45°C to avoid local pH fluctuations caused by temperature differences. Component A is put into the dynamic mixing tank 100 and stirred at a speed of 30 to 60 rpm to form a gentle vortex. Component B is injected into component A through multiple nozzles on the side wall of the dynamic mixing tank 100 at a flow rate of 0.4 to 0.8 L / min through the component B channel 200 to avoid liquid surface disturbance, and the online pH sensor is simultaneously turned on for real-time monitoring.
[0078] 2) Set the pH target range to 4.8-5.0. When the real-time pH is less than 4.8, add 0.5% triethanolamine through a metering pump at a gradient of 0.1%. If the pH is greater than 5.0, add citric acid buffer (pH=3.0) for fine adjustment to stabilize the pH of the initial mixed system within the range of 4.8-5.0.
[0079] Furthermore, the online pH sensor is installed at the bottom 1 / 3 height of the dynamic mixing tank 100 to avoid air bubble interference.
[0080] 3) During the initial mixing process, the temperature was controlled at 50-53°C to maintain the liposome liquid crystal phase (phase transition temperature 52°C) and prevent the collapse of the ceramide NP structure.
[0081] After the initial mixing is completed, the temperature is raised to 54-56°C, and 0.1% polyglycerol-10 laurate is preheated to 55°C and evenly dispersed into the mixing system in the form of a spray. Then, the anchor agitator in the dynamic mixing tank 100 is switched to a paddle type, and the diameter / pot diameter ratio of the paddle agitator is 0.4. The speed is increased to 80-100 rpm and maintained for 10-20 minutes to ensure uniform mixing while reducing the probability of liposome rupture in component B.
[0082] The above steps achieve efficient homogenization while protecting the structure of the active ingredients through laminar mixing and dynamic pH control. Component B is pumped in with laminar flow to reduce shear damage, and subsequent paddle stirring ensures microscopic homogenization, and the D90 particle size control accuracy is improved. In addition, the added polyglycerol-10 laurate forms a dense molecular film with a thickness of about 8nm at the oil-water interface at 55°C, which can effectively reduce the centrifugal stratification index of the mixed system and extend the shelf life stability to 24 months.
[0083] It is worth noting that when component B was mixed into component A, the mechanical impact energy was controlled below the critical rupture threshold of the liposome by laminar mixing, the encapsulation efficiency of ceramide NP was improved, and the lamellar liquid crystal structure was able to remain intact.
[0084] Step S4, preparation of component C.
[0085] Carbopol Ultrez 21 is a cross-linked polyacrylic acid polymer with a molecular weight of approximately 3×10 6 Da, swells under alkaline conditions (pH 5.0-6.5) to form a three-dimensional network gel structure. Propylene glycol is a dispersion medium used to reduce the agglomeration of Carbopol Ultrez 21 powder and partially neutralize the carboxylic acid group to promote pre-swelling.
[0086] The specific preparation method comprises: 1) Slowly add 0.25% Carbopol Ultrez 21 into propylene glycol with a solid-liquid ratio of 1:10 and stir at 500 rpm for 10 minutes to form a uniform suspension.
[0087] It is worth noting that the temperature of the stirring process is controlled at 22-28°C to avoid local gelation caused by high temperature.
[0088] 2) The suspension was allowed to stand for 30 min, and the particle size distribution was determined by laser diffraction. D50 increased from an initial 50 μm to 200 μm, and reached 300 μm after complete swelling, ensuring that the swelling rate was ≥ 95%. Swelling rate = volume after swelling / dry powder volume × 100%.
[0089] 3) The swollen fluid is injected into the mixing system through a static mixer. The static mixer blades divide, rotate and re-combine the fluid at a linear speed of 0.5 to 1 m / s and apply high-frequency shear for 1000 s. -1 , so that the Carbopol gel network is evenly embedded in the system to obtain component C, which has a viscosity of 4000-5000 CPS.
[0090] During the mixing process, the jacket was cooled (10°C circulating water) to maintain the system temperature <30°C to prevent excessive cross-linking of Carbopol.
[0091] Furthermore, a rotary online viscometer is installed at the outlet of the static mixer, and the data is fed back to the feed pump to adjust the flow rate. When the viscosity exceeds the range of 4000-5000 CPS, propylene glycol (to reduce viscosity) or Carbopol pregel (to increase viscosity) is automatically added.
[0092] Step S5: introduction and post-processing of functional additives.
[0093] Nitrogen bubbling deoxygenation, vacuum degassing and filtration are performed in sequence to obtain the olive essence.
[0094] Ethylhexylglycerin has the functions of preservative, synergistic and moisturizing. When adding, the temperature is controlled at ≤35℃, and it is slowly added dropwise after being pre-dissolved in 5% propylene glycol, with a stirring speed of 150rpm and a time of 10 minutes.
[0095] Tocopherol acetate is a fat-soluble antioxidant that scavenge lipid-phase free radicals and inhibit the oxidative degradation of olive polyphenols.
[0096] Nitrogen bubbling deoxygenation: It is preferred to use a porous titanium diffuser with a pore size of 10-20 μm and a nitrogen purity of ≥99.999%. During operation, the nitrogen flow rate is 2L / min, lasting for 30 minutes, and the temperature is controlled at 25-30°C to avoid low temperature causing increased viscosity and affecting bubble escape. Nitrogen bubbling deoxygenation can remove dissolved oxygen and prevent the oxidative degradation of active ingredients: olive polyphenols and ceramides.
[0097] Vacuum degassing: vacuum degree -0.095 MPa, maintain for 40 min, stirring speed 80 rpm. Those skilled in the art are familiar with the process and will not be described in detail here.
[0098] Filtration: It is preferred to use a double-layer nylon filter with a 5μm upper layer for pre-filtration and a 0.22μm lower layer for final filtration to effectively retain unentrapped free particles (such as Carbopol gel clumps, liposome fragments) and microbial load.
[0099] Through refined deoxygenation, degassing and terminal filtration, while ensuring the microbial safety and physical stability of the product, the efficacy of the active ingredients is retained to the greatest extent, ensuring the production quality of olive essence.
[0100] In summary, the present invention realizes "microenvironment customization" of active ingredients on a molecular scale through double encapsulation and isolation of salicylic acid and the combination of a dual buffer pair of disodium hydrogen phosphate (component A) and citric acid (component B), thereby achieving efficient coexistence of salicylic acid and ceramide, that is, salicylic acid maintains its activity at low pH (2.7-3.5), ceramide NP maintains its structure at neutral to acidic (5.0-5.8), and the pH of the system after mixing is stabilized at 4.8-5.0, thereby avoiding conflicts between components.
[0101] When component A (pH = 5.0-5.8) is mixed with component B (pH = 2.7-3.5), the two buffer systems achieve partition control and global stability through the following mechanisms: 1) Micro-level zone pH control: Phosphate buffer (HPO4 2- / H2PO4 - ) preferentially adsorbed on the liposome surface, maintaining the local pH ≈ 5.2, and the hydrophobic barrier of the liposome bilayer limits the H + Infiltration, protecting internal structures; Citric acid buffer (C6H8O7 / C6H5O7 - ) forms an acidic microenvironment (pH ≈ 3.5) around the mesoporous silica, and the HPβCD inclusion complex dissociates at low pH to release free salicylic acid.
[0102] 2) The buffering ranges of phosphate (pKa2=7.2) and citric acid (pKa1=3.1, pKa2=4.7, pKa3=6.4) partially overlap, forming a high buffering capacity platform (β≈0.05mol / pH) in the pH 4.8-5.0 range after mixing, resisting external acid-base interference; Triethanolamine dynamically neutralizes excess H + (free acid introduced by component B) to avoid a sudden drop in pH, while the citrate (C6H5O7 3- ) forms a complex with TEA to reduce alkalinity fluctuations.
[0103] The mixing effect of the olive essence prepared by the modulation and mixing method of the present invention is verified below.
[0104] Embodiment 1:
[0105] Based on the above olive essence preparation and mixing method, the olive essence is prepared, comprising the following steps: S1. Preparation of component A.
[0106] Mesoporous silica encapsulated olive polyphenols: Raw materials: crude extract of olive leaf polyphenols (oleuropein ≥ 10%, purity ≥ 80%); mesoporous silica (pore size 3nm, specific surface area 800m² / g, dried at 120℃ for 2h).
[0107] Olive polyphenols and mesoporous silica were mixed in a mass ratio of 1:2, anhydrous ethanol (solid-liquid ratio 1:10) was added, and stirred at 40°C for 2h; centrifugation (4000rpm, 15min) was performed to remove non-adsorbed polyphenols, and the precipitate was washed three times with deionized water; vacuum freeze-dried (-50°C, 24h) was performed to obtain drug-loaded particles (drug loading ≥15%, HPLC verification).
[0108] Preparation of phospholipid bilayer liposomes encapsulating ceramide NPs: Raw materials: hydrogenated soy lecithin (HSPC): cholesterol = 7:3 (mass ratio); ceramide NP (purity ≥ 95%), with total lipid mass ratio 1:5.
[0109] The lipids were dissolved in chloroform-methanol (2:1, v / v) and subjected to rotary evaporation (40°C, -0.08MPa) to form a film; hydrated with disodium hydrogen phosphate buffer (pH 5.5, 0.1M) containing 0.1% disodium EDTA, and oscillated at 55°C for 30 min; high-pressure homogenization (1000 bar, 3 cycles) was performed to obtain liposomes (D50=80±10nm, PDI<0.2).
[0110] Preparation of component A: Mix mesoporous silica drug-loaded particles and liposomes in a mass ratio of 1:9, add deionized water to a total solid content of 5%; stir at a low speed (200 rpm, 10 min) and then homogenize at a high speed (8000 rpm, 8 min), D90 = 140 nm; add 0.2% phytosterols, raise the temperature to 55°C and maintain for 15 min, and then gradually cool down to 40°C (rate 2°C / min) to obtain component A.
[0111] S2. Preparation of component B.
[0112] Preparation of salicylic acid-HPβCD inclusion complex: Hydroxypropyl-β-cyclodextrin (HPβCD, degree of substitution 0.8) was dissolved in 40% ethanol (solid-liquid ratio 1:15) and dissolved at 50°C; salicylic acid (molar ratio 1:2.5) was added, stirred for 6 hours in the dark, filtered and dialyzed (1000Da, 24 hours), and freeze-dried to obtain the inclusion complex.
[0113] Mesoporous silica secondary embedding: The inclusion complex was mixed with mesoporous silica (pore size 5 nm) in a mass ratio of 1:1, and adsorbed with the assistance of ultrasound (40 kHz, 200 W, 12 h); washed by centrifugation (5000 rpm, 20 min), and dried in vacuum at 40°C to obtain secondary embedded particles.
[0114] Preparation of component B: premix the embedded particles with 5% PCA zinc (purity ≥98%) in glycerol, add citric acid buffer (pH 3.0, 0.1M); stir at low speed (200rpm, 25min), free salicylic acid concentration ≤0.1% (HPLC detection, add 0.5% HPβCD if exceeding the standard).
[0115] S3, the diameter of the B component channel 200 is set to 6mm, and 4 nozzles are evenly distributed on the side wall of the dynamic mixing tank 100. The B component is pumped into the A component in a laminar flow mode, and the anchor stirrer is used to slowly stir, and the Reynolds number in the initial mixing is maintained at 1600-1800, and the mixing temperature is controlled at 52°C. In addition, the pH is adjusted to 4.9 online (triethanolamine supplementary acceleration 0.1% / min). After the initial mixing is completed, that is, 5 minutes after the corresponding B component is completely pumped in, the fluid temperature is raised to 55°C, and 0.1% polyglycerol-10 laurate (preheated to 55°C) is added; the paddle stirrer is switched to stir at 80rpm for 12 minutes to obtain a mixed system.
[0116] S4, disperse 0.25% Carbopol Ultrez 21 in propylene glycol (solid-liquid ratio 1:10), stir at 25℃ for 10min, let it swell for 30min, swelling ratio ≥95% (laser diffraction method verifies D50=200μm). -1 ) injection system; online viscometer monitoring, adjust to the viscosity of 4500±200cPs (25℃, Brookfield RV).
[0117] S5. Add 0.5% ethylhexylglycerol (pre-dissolved in 5% propylene glycol) and 0.1% tocopherol acetate; stir at 35°C at a low speed (150 rpm, 10 min). Nitrogen bubbling deoxygenation (2 L / min, 30 min, dissolved oxygen ≤ 1 ppm); vacuum degassing (-0.095 MPa, 40 min, bubble diameter ≤ 20 μm). Terminal filtration: double-layer nylon filter membrane (5 μm pre-filtration + 0.22 μm final filtration) to intercept free particles and microorganisms to prepare the olive essence of this embodiment.
[0118] Based on Example 1, a control experiment was designed as shown in Table 1: Table 1. Experimental groups
[0119] The above experimental groups were tested for antioxidant, moisturizing, acne removal, barrier repair and safety: Antioxidant: DPPH free radical scavenging rate (GB / T 27500-2011); Moisturizing: Corneometer® CM825 (ISO 24444:2019); Acne removal: Propionibacterium acnes inhibition test (CLSI M11-A8); Barrier repair: in vitro skin model (Franz diffusion cell); Safety: human patch test (ISO 10993-10).
[0120] The results of the comparative experiment are as follows: the DPPH clearance rate of Example 1 and the control group 1 is greater than 90%, which has a good antioxidant effect; the 24h stratum corneum water content of Example 1 is increased by 26.4%, and the control group 1 is increased by 28.9%, and the moisturizing effect is slightly lower than that of the control group 1, but higher than 24.3% of the control group 2; Example 1 and the control group 2 have the same effect, both of which are MIC≤0.5μg / mL, and the acne removal effect is similar; the ceramide NP penetration of Example 1 is 8.2μg / cm², and the salicylic acid rate is 0.85μg / (cm²·h); The allergy rate of Example 1 is less than 3%, which meets the safety standards of cosmetics.
[0121] It can be seen that the olive essence prepared by Example 1 of the present invention has three major effects: anti-oxidation, moisturizing and acne removal: Antioxidant: The serum contains olive polyphenols, which have strong antioxidant capacity, can scavenge free radicals and inhibit lipid peroxidation. Olive polyphenols are encapsulated by mesoporous silica, which not only protects olive polyphenols from oxidative degradation, but also controls their slow release process, thereby enhancing tolerance to acidic environments.
[0122] Moisturizing: Ceramide NP as the core moisturizing ingredient is encapsulated by phospholipid bilayer liposomes. This structure helps to replenish lipids in the stratum corneum, repair the skin barrier, and enhance transdermal efficiency. At the same time, the liposome maintains the stability of the liquid crystal structure, adapts to the pH value between 5.0 and 5.8, matches the physiological environment, and prevents the risk of stratification. In addition, the addition of phytosterols further enhances the moisturizing time and improves the tolerance of the ceramide NP liquid crystal structure to pH.
[0123] Acne treatment: Salicylic acid, as an effective acne treatment ingredient, is combined with hydroxypropyl-β-cyclodextrin (HPβCD) through mesoporous silica secondary embedding technology to form an inclusion complex and then undergo secondary embedding. This method ensures that salicylic acid can be released from mesoporous silica in a low pH environment (less than 3.5) and act specifically on the acidic microenvironment of acne lesions. PCA zinc is also added to the formula, which not only controls oil and locks in moisture, but also inhibits the growth of Propionibacterium acnes, assisting in the acne treatment effect.
[0124] In addition, in order to ensure that each active ingredient can maintain its characteristics and efficacy during the mixing process, a citric acid-disodium hydrogen phosphate dual buffer system is used to control the pH value in different areas. This strategy ensures that salicylic acid remains active under low pH conditions while avoiding affecting the stability of ceramide NP. The essence finally prepared covers the needs of anti-oxidation, moisturizing and acne removal, can effectively remove red blood streaks, inhibit acne regeneration, fade acne marks, and repair damaged skin, helping to restore the skin to its natural and healthy state.
[0125] The following is an experiment on the influence of the mixing process control of component A and component B in step S3 on the preparation and mixing effect of olive essence.
[0126] Based on Example 1, seven groups were designed for comparative experiments, as shown in Table 2: Table 2. Modulation and mixing experiments
[0127] The test indicators of this experiment include: ceramide encapsulation rate (%), salicylic acid free concentration (%), centrifugal stratification index (%), transdermal efficiency (ceramide, μg / cm²), transdermal efficiency (salicylic acid, μg / (cm²·h)) and viscosity stability (6 weeks, %).
[0128] The Reynolds number of group G is too low, the mixing effect is not up to standard, and the mixing time is too long.
[0129] The specific experimental results are shown in Table 3 below: Table 3. Summary of modulation mixing experiment results
[0130] The analysis of the results of the modulation mixing experiment showed that pH value had a significant effect on the mixing effect. At pH 4.8 (group A) and pH 5.0 (group B), the ceramide encapsulation efficiency exceeded 90%, the free salicylic acid concentration did not exceed 0.1%, and the centrifugal stratification index was less than 4%, which was due to the synergistic effect of the double buffer between pH 4.8 and 5.0: the sodium hydrogen phosphate buffer maintained the pH of the liposome surface at about 5.2 to protect the ceramide liquid crystal structure; the citric acid buffer formed an acidic microenvironment of about pH 3.5 around the mesoporous silica to promote the release of salicylic acid; triethanolamine neutralized the free acid to prevent a sudden drop in pH. However, at pH 5.5 (group C), the encapsulation efficiency dropped to 75.3% and the stratification index increased to 12.4%, indicating that when the pH was higher than 5.0, the sodium hydrogen phosphate buffer capacity decreased, resulting in a weakened barrier effect of the liposome bilayer membrane and a partial disintegration of the ceramide liquid crystal structure. Similarly, at pH 4.0 (group D), since the citric acid buffer dominated the system, the excessive acidity destroyed the stability of the liposomes, resulting in a free salicylic acid concentration as high as 0.25% and a stratification index of 18.6%.
[0131] The Reynolds number of the mixing process also affects the mixing effect. At Re≈1800 (Group A), the ceramide transdermal efficiency reached 8.2μg / cm², and the salicylic acid transdermal rate was 0.85μg / (cm²·h), proving that the advantage of laminar mixing (Re=1000-2000) is that the shear force is lower than the critical rupture threshold of the liposome, protecting the encapsulation rate and avoiding premature release caused by turbulence. At Re≈2500 (Group E) and Re≈4000 (Group F), the encapsulation rate dropped to 84.2% and 71.6%, respectively, and the stratification index increased, indicating that the turbulent shear force generated by the high Reynolds number damaged the liposome bilayer membrane and caused the aggregation of mesoporous silica particles, reducing the sustained release efficiency. On the contrary, at Re≈800 (Group G), despite the low Reynolds number, the stratification index was as high as 23.1% due to insufficient mixing, uneven distribution, and unstable oil-water interface film, and the transdermal efficiency was significantly reduced.
[0132] In summary, the best performance was achieved in Group A, which not only achieved a ceramide encapsulation rate of 92.5% and a free salicylic acid concentration of 0.08%, but also demonstrated good transdermal efficiency and viscosity stability, as well as a low centrifugal stratification index of 3.2%, verifying the effectiveness of pH zoning control, double embedding technology, and static mixer design. Experimental data show that through precise pH control (4.8-5.0) and Reynolds number control (1000-2000), the method of the present invention can optimize the industrial production of multi-effect essences, providing antioxidant, moisturizing, and anti-acne effects.
[0133] like Figure 3 As shown, the present invention also provides an olive essence mixing device, comprising: a mixing mechanism, including a dynamic mixing tank 100, and a three-channel dosing component arranged on the dynamic mixing tank 100; the dynamic mixing tank 100 is used to mix component A and component B; a gel mechanism, used for pre-gelling Carbopol Ultrez 21 and propylene glycol; a static mixer, used to inject the pre-gel into the main mixing system; an injection pump, connected to the static mixer, respectively pumping the main mixing system and the pre-gel into the static mixer; and a post-treatment component, including a nitrogen bubbling tower, a vacuum degassing tank and a filter element.
[0134] It is worth noting that the three-channel dosing assembly includes: a B component channel 200, which is configured as a plurality of pipe openings surrounding the side wall of the dynamic mixing tank 100, and the direction of the pipe openings is consistent with the rotation direction of the agitator in the dynamic mixing tank 100; a pH adjustment channel 300, which is arranged at the upper part of the dynamic mixing tank 100; and an additive channel 400, which is arranged at the upper part of the dynamic mixing tank 100.
[0135] The special arrangement of the B component channel 200 can ensure that the Reynolds number is within the range of 1000-2000 when the A component and the B component are mixed, while also accelerating the mixing efficiency.
[0136] Furthermore, the dynamic mixing tank 100 is also provided with a temperature control module and a stirring assembly for controlling the temperature and stirring the mixing system during mixing, wherein the stirring paddle of the stirring assembly is detachable and replaceable, which will not be elaborated in detail here.
[0137] The above is based on the ideal embodiment of the present invention. Through the above description, relevant personnel can make various changes and modifications without departing from the technical concept of the present invention. The technical scope of the present invention is not limited to the content in the specification, and the technical scope must be determined according to the scope of the claims.
Claims
1. A method for preparing and mixing olive essence, characterized in that: The following steps are involved: S1. Mixing olive polyphenols encapsulated by mesoporous silica with ceramide NPs encapsulated by phospholipid bilayer liposomes, adding disodium hydrogen phosphate buffer to adjust the pH value to 5.0-5.8, stirring at a low speed and then homogenizing at a high speed, adding phytosterols simultaneously, and heating to 50-60° C. for 10-20 min, and cooling to obtain component A; S2, mixing the salicylic acid-HPβCD inclusion complex embedded in mesoporous silica with PCA zinc in glycerol, adjusting the pH value to 2.7-3.5 by adding citric acid buffer, and stirring at a low speed for 20-30 minutes to obtain component B; S3, preliminarily mix component B and component A, add triethanolamine simultaneously, keep the mixing temperature at 50-53°C, and control the pH value between 4.8 and 5.0; After the initial mixing is completed, polyglycerol-10 laurate is added and stirred continuously at 54-58°C for 10-20 minutes to form a mixed system; S4, pre-gelling Carbopol Ultrez 21 and propylene glycol, and injecting them into the mixed system through a static mixer to generate component C; S5. After adding ethylhexylglycerol and tocopherol acetate to component C, nitrogen bubbling deoxygenation, vacuum degassing and filtration are performed in sequence to obtain the olive essence.
2. The method for preparing and mixing olive essence according to claim 1, characterized in that: In S3, the Reynolds number of the preliminary mixing process is controlled within the range of 1000 to 2000.
3. The method for preparing and mixing olive essence according to claim 1, characterized in that: In the above S3, when the B component is pumped into the A component, the diameter of the B component channel pipe used is 4-7 mm, and the flow rate of the B component is 0.4-0.8 L / min.
4. The method for preparing and mixing olive essence according to claim 1, characterized in that: In S1, the low-speed stirring rate is 100-300 rpm, and the time is 5-15 min; The high-speed homogenization rate is 7000-9000rpm, and D90 after homogenization is less than 150nm.
5. The method for preparing and mixing olive essence according to claim 1, characterized in that: In S2, the preparation method of mesoporous silica secondary embedding salicylic acid-HPβCD inclusion complex comprises: S21, including salicylic acid and hydroxypropyl-β-cyclodextrin in a molar ratio of 1:2 to 3; S22. Using mesoporous silica to perform secondary encapsulation of the salicylic acid-HPβCD inclusion complex prepared in S21.
6. The method for preparing and mixing olive essence according to claim 1, characterized in that: In the S1, the mass ratio of the mesoporous silica-encapsulated olive polyphenol and the phospholipid bilayer liposome-encapsulated ceramide NP when mixed is 0.5-2:
9.
7. The method for preparing and mixing olive essence according to claim 1, characterized in that: In S4, the control parameters of the static mixer are: linear velocity of 0.5-1 m / s, shear rate of 800-1200 s -1 .
8. The method for preparing and mixing olive essence according to claim 1, characterized in that: In S3, triethanolamine is dynamically added through an online sensor to ensure that the pH value of the preliminary mixed system is stabilized between 4.8 and 5.
0.
9. An olive essence preparation and mixing device, used in the olive essence preparation and mixing method according to any one of claims 1 to 8, characterized in that: include: A mixing mechanism, comprising a dynamic mixing tank, and a three-channel dosing assembly arranged on the dynamic mixing tank; The dynamic mixing tank is used for mixing component A and component B; Gel mechanism for pre-gelling of Carbopol Ultrez 21 with propylene glycol; Static mixer, used to inject pre-gel into the main mixing system; An injection pump is connected to the static mixer to pump the main mixing system and the pre-gel into the static mixer respectively; And post-processing components, including nitrogen bubbling tower, vacuum degassing tank and filter element.
10. The olive essence preparation and mixing device according to claim 9, characterized in that: The three-channel dosing assembly comprises: A component B channel configured as a plurality of orifices surrounding the side wall of the dynamic mixing tank; A pH adjustment channel is arranged at the upper part of the dynamic mixing tank; The additive channel is arranged at the upper part of the dynamic mixing tank.
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