Microorganism and nucleic acid removal material based on high-temperature stable sustained-release microspheres, preparation method of microorganism and nucleic acid removal material and application of microorganism and nucleic acid removal material in high-temperature condition

Abstract

The invention relates to the technical field of disinfectants, in particular to a microorganism and nucleic acid removal material based on high-temperature stable sustained-release microspheres, a preparation method of the microorganism and nucleic acid removal material and application of the microorganism and nucleic acid removal material in a high-temperature condition. The microorganism and nucleic acid removal material based on the high-temperature stable sustained-release microspheres is prepared from an oil phase raw material, an inner water phase raw material and an outer water phase, the oil phase raw material comprises poly-L-lactic acid; the inner water phase raw material is a mixture of a cationic polymer and benzalkonium chloride; the cationic polymer comprises any two or three of polyhexamethylene biguanide, polyethyleneimine and chitosan. According to the invention, by optimizing the formula of the microorganism and nucleic acid removal material based on the high-temperature stable sustained-release microspheres, multiple advantages of high-temperature stability, efficient nucleic acid inactivation, accurate release, environmental friendliness, long-acting disinfection and the like are realized, and a brand-new, efficient and reliable solution is provided for the disinfection demand in a high-temperature environment.

Description

Technical Field

[0001] This invention relates to the field of disinfectant technology, and in particular to a microbial and nucleic acid removal material based on high-temperature stable slow-release microspheres, its preparation method, and its application under high-temperature conditions. Background Technology

[0002] In the field of disinfection, factors such as air humidity, ambient temperature, climate conditions, and air pressure all affect the disinfection effectiveness of disinfectants to some extent. Traditional disinfectants have poor stability at high temperatures, making it difficult for them to effectively disinfect and sterilize. For example, the active ingredients in common chlorine-containing disinfectants are easily decomposed under high temperatures, resulting in a significant reduction in disinfection effectiveness. While some high-temperature disinfection methods, such as high-temperature steam sterilization, can effectively kill microorganisms, they cannot destroy the nucleic acids of specific microorganisms, posing a certain risk of transmission.

[0003] Furthermore, while some existing microsphere disinfectants possess certain slow-release properties and sterilization effects, their stability under high-temperature conditions remains unsatisfactory. For example, although potassium persulfate microspheres exhibit good bactericidal effects against Escherichia coli and Staphylococcus aureus, the release rate and stability of their active ingredients under high-temperature conditions still require further optimization. Simultaneously, these microsphere disinfectants often only disrupt the cellular structure of microorganisms through physical or chemical actions, failing to penetrate to the nucleic acid level for complete inactivation.

[0004] Therefore, developing a microsphere disinfectant that can exist stably under high temperature conditions and effectively kill microbial nucleic acids is of great significance for improving disinfection effects and eliminating the risk of microbial transmission. Summary of the Invention

[0005] This invention provides a microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres, its preparation method, and its application under high-temperature conditions, in order to solve the above-mentioned defects in the prior art, thereby obtaining a microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres that can exist stably under high-temperature conditions and can effectively kill microbial nucleic acids.

[0006] The present invention has the following technical solution: This invention provides a microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres. The microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres is mainly prepared from an oil phase raw material, an inner aqueous phase raw material, and an outer aqueous phase. The oil phase raw material includes poly-L-lactic acid. The inner aqueous phase raw material is a mixture of cationic polymer, polyhexamethylene biguanide, and benzalkonium chloride. The cationic polymer includes any two or three of polyhexamethylene biguanide, polyethyleneimine, and chitosan.

[0007] This invention optimizes the formulation of disinfectants, greatly improving the stability of microbial and nucleic acid removal materials based on high-temperature stable slow-release microspheres, enabling them to exist stably under high-temperature conditions and effectively solving the problem of traditional disinfectants decomposing and failing under high-temperature environments.

[0008] In particular, traditional disinfectants are unstable at high temperatures and easily degrade and become ineffective. For example, in scenarios requiring high-temperature disinfection such as homes, restaurants, and hotels, as well as in hospitals, feed filling pipelines, summer farms, and areas where surfaces may experience high temperatures after disease outbreaks, nucleic acid testing is used to confirm complete disinfection. Conventional disinfectants show a sharp decrease in effectiveness at high temperatures, thus necessitating the use of high-temperature disinfectants. However, the microbial and nucleic acid removal material based on high-temperature stable slow-release microspheres obtained by this invention maintains excellent bactericidal and disinfection effects under high-temperature conditions. This makes the product suitable for occasions requiring high-temperature disinfection, such as tableware. By using this heat-resistant disinfectant, disinfection effectiveness under high-temperature conditions can be effectively guaranteed.

[0009] According to the present invention, a microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres is provided, wherein the cationic polymer is a mixture of polyhexamethylene biguanide and polyethyleneimine.

[0010] According to the present invention, a microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres is provided, wherein the mass ratio of polyhexamethylene biguanide and polyethyleneimine in the cationic polymer is (1~4):(1~4), for example, it can be any ratio among 1:1, 1:2, 1:3, 1:4, 4:1, 3:1, 2:1, or any ratio range with any two of the above ratios as endpoints.

[0011] In this invention, a mixture of polyethyleneimine and polyhexamethylene biguanide is preferably used as a cationic polymer. Polyethyleneimine is a cationic polymer widely used in nucleic acid delivery. However, this application found that when it is applied in the system of this application, it can efficiently and effectively kill nucleic acids. The disinfection mechanism mainly lies in the fact that the cations pierce the cell wall, cell membrane and viral cell membrane of bacteria, and deliver effective substances into the cell for efficient disinfection.

[0012] In this invention, the molecular weight of the poly-L-lactic acid can be between 50,000 and 100,000, for example, any value among 50,000, 55,000, 60,000, 65,000, 70,000, 75,000, 80,000, 85,000, 90,000, 95,000, and 100,000, or a range of values ​​with any two of the above values ​​as endpoints; the molecular weight of the polyethyleneimine can be between 3,000 and 20,000, for example, any value among 3,000, 4,000, 5,000, 6,000, 7,000, 8,000, 9,000, 10,000, 11,000, 12,000, 13,000, 14,000, 15,000, 16,000, 17,000, 18,000, 19,000, and 20,000, or a range of values ​​with any two of the above values ​​as endpoints.

[0013] According to the present invention, a microbial and nucleic acid scavenging material based on high-temperature stable slow-release microspheres is provided, wherein the content of polyethyleneimine in the internal aqueous phase raw material is 1wt% to 25wt%; for example, it can be any value among 1wt%, 2wt%, 3wt%, 4wt%, 5wt%, 6wt%, 7wt%, 8wt%, 9wt%, 10wt%, 11wt%, 12wt%, 13wt%, 14wt%, 15wt%, 16wt%, 17wt%, 18wt%, 19wt%, 20wt%, 21wt%, 22wt%, 23wt%, 24wt%, and 25wt%, or a range of values ​​with any two of the above values ​​as endpoints.

[0014] This invention discovers that the aqueous raw material of the microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres contains the aforementioned amount of polyethyleneimine, which is more conducive to enhancing the synergistic effect of the components. The resulting microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres can penetrate deep into the interior of microorganisms and directly act on their nucleic acids. By destroying their nucleic acid structure, it completely kills the microorganisms, thereby completely eliminating the risk of microbial transmission. Compared with traditional disinfectants that only destroy the microbial cell structure, the disinfectant of this application inactivates at the nucleic acid level, resulting in a more thorough disinfection effect. It can effectively deal with drug-resistant strains and difficult-to-kill microorganisms, providing a more reliable guarantee for public health safety.

[0015] According to the present invention, a microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres is provided, wherein the inner aqueous phase raw material is a mixture of cationic polymer and benzalkonium chloride in a mass ratio of (2~5):(2~4). This ratio helps to ensure that each component in the inner aqueous phase raw material fully exerts its function, synergistically with the oil phase raw material, and enhances the nucleic acid-destructive ability of the high-temperature stable sustained-release microsphere-based microbial and nucleic acid removal material. Simultaneously, this limited ratio also helps to better control the amount of raw materials added during the preparation process, ensuring that the preparation process of the high-temperature stable sustained-release microsphere-based microbial and nucleic acid removal material is stable and controllable, thereby guaranteeing the quality and performance of the final product.

[0016] According to the present invention, a microbial and nucleic acid removal material based on high-temperature stable slow-release microspheres is provided, wherein the volume ratio of the oil phase raw material to the internal aqueous phase raw material is 1:(3~5).

[0017] In some specific embodiments, the volume ratio of the oil phase raw material to the internal aqueous phase raw material can be any ratio among 1:3, 1:4, and 1:5, or a range of ratios with any two of the above ratios as endpoints.

[0018] In this invention, the particle size of the microbial and nucleic acid scavenging material based on high-temperature stable sustained-release microspheres is 1µm to 20µm. For example, it can be any value among 1µm, 2µm, 3µm, 4µm, 5µm, 6µm, 7µm, 8µm, 9µm, 10µm, 11µm, 12µm, 13µm, 14µm, 15µm, 16µm, 17µm, 18µm, 19µm, and 20µm, or a range of values ​​with any two of the above values ​​as endpoints.

[0019] Secondly, the present invention provides a method for preparing microbial and nucleic acid scavenging materials based on high-temperature stable sustained-release microspheres, wherein the microsphere preparation system is used to prepare microbial and nucleic acid scavenging materials based on high-temperature stable sustained-release microspheres. The microsphere preparation system includes a membrane emulsification device (210); the membrane emulsification device (210) includes a plurality of filter membranes (211), which are arranged in parallel; an outer flow channel (212) is formed between two adjacent filter membranes (211); an inner flow channel (213) is formed in the filter membrane (211) along its own axial direction, and a plurality of micropores (214) are opened on the tube wall of the filter membrane (211), and the outer flow channel (212) is connected to the inner flow channel (213) through the micropores (214).

[0020] Preferably, the membrane emulsification device (210) further includes: a dispersed phase supply device (220) and an external aqueous phase supply device (230); the dispersed phase supply device (220) is connected to the external flow channel (212) and is used to inject the dispersed phase into the external flow channel (212); the external aqueous phase supply device (230) is connected to the internal flow channel (213) to form an external aqueous phase circulation loop.

[0021] The dispersed phase supply device (220) includes a first dispersed phase storage unit (221), a second dispersed phase storage unit (222), and a first valve body unit (223); both the first dispersed phase storage unit (221) and the second dispersed phase storage unit (222) are used to store the dispersed phase; the first valve body unit (223) has a first conducting state and a second conducting state; in the first conducting state, the first dispersed phase storage unit (221) injects the dispersed phase into the external flow channel (212); in the second conducting state, the second dispersed phase storage unit (222) injects the dispersed phase into the external flow channel (212); the first valve body unit (223) includes a first three-way valve, and the external flow channel (212) is connected to the first dispersed phase storage unit (221) and the second dispersed phase storage unit (222) respectively through the first three-way valve.

[0022] The external water phase supply device (230) includes an external water phase storage module (231) and a circulation power source (232); the external water phase storage module (231) is used to store the external water phase; the inlet of the external water phase storage module (231) is connected to the outlet of the inner flow channel (213), and the outlet of the external water phase supply device (230) is connected to the inlet of the inner flow channel (213) to form the external water phase circulation loop; the circulation power source (232) is located in the external water phase circulation loop.

[0023] The external water phase storage module (231) includes a first external water phase storage unit (2311), a second external water phase storage unit (2312), and a second valve body unit; both the first external water phase storage unit (2311) and the second external water phase storage unit (2312) are used to store the external water phase; the second valve body unit has a third conducting state and a fourth conducting state; in the third conducting state, the first external water phase storage unit (2311) injects the external water phase into the inner flow channel (213); in the fourth conducting state, the second external water phase storage unit (2312) injects the external water phase into the inner flow channel (213). The inner flow channel (213) is used to inject the external water phase; the second valve body unit includes a second three-way valve (2313) and a fourth three-way valve (2314); the inlet of the inner flow channel (213) is connected to the outlet of the first external water phase storage unit (2311) and the outlet of the second external water phase storage unit (2312) through the second three-way valve (2313); the outlet of the inner flow channel (213) is connected to the inlet of the first external water phase storage unit (2311) and the inlet of the second external water phase storage unit (2312) through the fourth three-way valve (2314).

[0024] Preferably, the membrane emulsification device (210) further includes an emulsion storage device (240), which is connected to the inner flow channel (213) and is used to store the emulsion discharged from the inner flow channel (213).

[0025] Preferably, the membrane emulsification device (210) further includes a pressure supply device (250) connected to the outer channel (212) for introducing protective gas into the outer channel (212) to push the dispersed phase through the micropores (214) to form emulsion droplets in the inner channel (213).

[0026] According to the present invention, a method for preparing microbial and nucleic acid scavenging materials based on high-temperature stable sustained-release microspheres is provided, the preparation method comprising the following steps: S1: The first surfactant is mixed with water to obtain the outer aqueous phase; the inner aqueous phase raw material is mixed with the second surfactant to obtain the inner aqueous phase; the oil phase raw material is dissolved in an organic solvent to obtain an oil phase solution; then the inner aqueous phase and the oil phase solution are mixed, and the water-in-oil emulsion obtained by ultrasonication is the dispersed phase; S2: Inject the dispersed phase into the outer channel (212) and inject the outer aqueous phase into the inner channel (213); introduce protective gas into the outer channel (212) to push the dispersed phase through the micropores (214) to form droplets in the inner channel (213) and mix with the outer aqueous phase to form an emulsion; S3: The emulsion is dried and then subjected to high-temperature complexation; preferably, the high-temperature complexation temperature is 80℃~100℃, for example, it can be any value among 80℃, 81℃, 82℃, 83℃, 84℃, 85℃, 86℃, 87℃, 88℃, 89℃, 90℃, 91℃, 92℃, 93℃, 94℃, 95℃, 96℃, 97℃, 98℃, 99℃, 100℃, or a range of values ​​with any two of the above values ​​as endpoints.

[0027] According to the present invention, a method for preparing microbial and nucleic acid scavenging materials based on high-temperature stable sustained-release microspheres is provided. The first surfactant and the second surfactant each independently, identically, or differently comprise polyvinyl alcohol and / or hexadecyltrimethylammonium bromide. The concentration of the first surfactant in the external aqueous phase is 0.5wt% to 1.5wt%, for example, any value among 0.5wt%, 0.6wt%, 0.7wt%, 0.8wt%, 0.9wt%, 1.0wt%, 1.1wt%, 1.2wt%, 1.3wt%, 1.4wt%, and 1.5wt%, or a range of values ​​with any two of the above values ​​as endpoints. The concentration of the second surfactant in the internal aqueous phase is 0.5wt% to 1.5wt%, for example, any value among 0.5wt%, 0.6wt%, 0.7wt%, 0.8wt%, 0.9wt%, 1.0wt%, 1.1wt%, 1.2wt%, 1.3wt%, 1.4wt%, and 1.5wt%, or a range of values ​​with any two of the above values ​​as endpoints.

[0028] The present invention has found that the above-mentioned surfactant can improve the stability of the aqueous phase and prevent the aggregation of PLA microspheres.

[0029] According to the present invention, a method for preparing microbial and nucleic acid removal materials based on high-temperature stable sustained-release microspheres is provided, wherein the organic solvent includes dichloromethane.

[0030] According to the present invention, a method for preparing microbial and nucleic acid removal materials based on high-temperature stable sustained-release microspheres is provided, wherein the mass ratio of the inner aqueous phase and the oil phase solution is 1:(5~10); for example, it can be any ratio among 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, or any ratio range with any two of the above ratios as endpoints.

[0031] In this invention, the microbial and nucleic acid removal materials based on high-temperature stable sustained-release microspheres prepared by the above system and method are beneficial for precise control of particle size and particle size distribution. The PDI is much lower than the pharmaceutical standard requirement of 0.2, and it can realize the batch synthesis of liposome microspheres, breaking through the bottleneck of large-scale microsphere preparation.

[0032] Thirdly, the application of the microbial and nucleic acid removal material based on high-temperature stable slow-release microspheres described in this invention under high-temperature conditions; preferably, the temperature of the high-temperature conditions is 50~95℃.

[0033] The microbial and nucleic acid removal material based on high-temperature stable slow-release microspheres described in this invention can maintain high-efficiency disinfection performance in high-temperature environments or during high-temperature disinfection processes, which greatly expands its application scenarios, such as in food processing, high-temperature disinfection of medical equipment, and hygiene and epidemic prevention in high-temperature environments.

[0034] According to the present invention, the application of the microbial and nucleic acid removal material based on high-temperature stable slow-release microspheres in high-temperature conditions can be achieved by preparing the microbial and nucleic acid removal material based on high-temperature stable slow-release microspheres into an aqueous solution of 0.001wt%~0.01wt% according to the application scenario and spraying it directly onto the surface of the object.

[0035] Fourthly, the present invention provides a disinfection product containing the aforementioned microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres; preferably, the content of the microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres in the disinfection product is 0.001wt%~0.01wt%; that is, this concentration range can effectively kill microorganisms and remove viral nucleic acids. For example, it can be any value from 0.001wt%, 0.002wt%, 0.003wt%, 0.004wt%, 0.005wt%, 0.006wt%, 0.007wt%, 0.008wt%, 0.009wt%, 0.01wt%, or a value range with any two of the above values ​​as endpoints, preferably 0.001wt%~0.005wt%.

[0036] Based on this, the present invention has the following technical solution: This invention optimizes the formulation of microbial and nucleic acid removal materials based on high-temperature stable slow-release microspheres, achieving multiple advantages such as high-temperature stability, efficient nucleic acid inactivation, precise release, environmental friendliness, and long-lasting disinfection, providing a new, efficient, and reliable solution for disinfection needs in high-temperature environments. Attached Figure Description

[0037] To more clearly illustrate the technical solutions in this invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0038] Figure 1This is a schematic diagram of the preparation system for microbial and nucleic acid removal materials based on high-temperature stable sustained-release microspheres provided by the present invention.

[0039] Figure 2 This is a top-view structural schematic diagram of the membrane emulsification device of the preparation system for microorganisms and nucleic acid removal materials based on high-temperature stable slow-release microspheres provided by the present invention.

[0040] Figure 3 This is a schematic diagram of the filter membrane structure of the membrane emulsification device provided by the present invention.

[0041] Figure 4 yes Figure 3 A magnified structural diagram of point A in the middle.

[0042] Figure 5 This is a flowchart of the preparation method of microbial and nucleic acid removal materials based on high-temperature stable sustained-release microspheres provided by the present invention.

[0043] Figure 6 This is a schematic diagram of a filter membrane processing system based on a traditional Bessel beam.

[0044] Figure 7 This is a schematic diagram of the filter membrane processing system provided by the present invention.

[0045] Figure 8 This is a schematic diagram illustrating the principle of the reflective axial pyramid provided by the present invention reflecting incident light rays to form a Bessel beam; wherein, The reflectivity of the reflective axial pyramid. The base angle of the reflective axial pyramid. The diffraction angle of the Bessel region; The focal depth of the non-diffraction region of the Bessel beam; Represents the incident laser. The wavelength representing the incident laser light. Represents the radius of the incident laser beam.

[0046] Figure 9 It is the image of the incident laser after passing through the reflective axial pyramid and the spot image at the processing station.

[0047] Figure 10 These are simulation diagrams of the transverse and longitudinal light intensity distribution of Bessel and Gaussian beams: (a) and (b) are simulation diagrams of the light field of the Bessel beam; (c) and (d) are simulation diagrams of the light field of the Gaussian beam.

[0048] Figure 11 This invention describes the use of a filter membrane processing system to create 1-micron pores in stainless steel.

[0049] Figure 12This is a transmission electron microscope image of a high-temperature stable sustained-release microsphere-based microbial and nucleic acid removal material suitable for high-temperature conditions, as provided in Example 1 of this invention.

[0050] Figure 13 This is a diagram showing the bactericidal effect of the high-temperature stable slow-release microsphere-based microbial and nucleic acid removal material, which is suitable for high-temperature conditions, on Escherichia coli within 1 minute after high-temperature treatment, according to Example 1 of the present invention.

[0051] Figure 14 This is a diagram showing the bactericidal effect of the high-temperature stable slow-release microsphere-based microbial and nucleic acid removal material, which is suitable for high-temperature conditions, on Escherichia coli within 4 weeks after high-temperature treatment, according to Example 1 of the present invention.

[0052] Figure label: 110. Beam shaping assembly; 120. Transmission assembly; 121. Lens; 122. Field lens; 130. Galvanometer assembly; 140. Beam expander; 150. Polarization assembly; 151. Half-wave plate; 152. Polarizer; 160. Laser source; 170. Mirror; 210. Membrane emulsification device; 211. Filter membrane; 212. External flow channel; 213. Internal flow channel; 214. Micropores; 215. Outer shell; 220. Dispersed phase supply device; 221. First dispersed phase storage unit; 222. Second dispersed phase storage unit; 223. First valve body unit; 230. External water phase supply device; 231. External water phase storage module; 2311. First external water phase storage unit; 2312. Second external water phase storage unit; 2313. Second three-way valve; 2314. Fourth three-way valve; 232. Circulation power source; 2321. Circulation pump; 2322. Flow detection unit; 240. Emulsion storage device; 250. Pressure supply device; 251. Air pump; 252. Pressure gauge; 253. Third three-way valve; 254. Sixth three-way valve; 260. Third valve body unit. Detailed Implementation

[0053] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this invention. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without creative effort are within the scope of protection of this invention.

[0054] The following is combined Figures 1 to 4The present invention provides a detailed description of the preparation system and working principle of the microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres.

[0055] like Figures 1 to 4 As shown, a specific embodiment of the first aspect of the present invention provides a preparation system for microbial and nucleic acid removal materials based on high-temperature stable sustained-release microspheres. The preparation system includes a membrane emulsification device 210; the membrane emulsification device 210 includes multiple filter membranes 211; the multiple filter membranes 211 are arranged in parallel; an external flow channel 212 is formed between two adjacent filter membranes 211; an internal flow channel 213 is formed within the filter membrane 211 along its own axial direction; multiple micropores 214 are formed on the wall of the filter membrane 211; the external flow channel 212 communicates with the internal flow channel 213 through the micropores 214.

[0056] In this embodiment, by arranging multiple filter membranes 211 in parallel, a large amount of raw materials can be processed simultaneously, significantly increasing the microsphere yield per unit time. This overcomes the bottleneck of low efficiency in traditional single filter membranes, making it suitable for industrial-scale production. It also solves the problem of limited output of existing membrane emulsification devices 210, which require multiple devices 210 to participate simultaneously in the emulsification process in large-scale emulsification scenarios, leading to high costs. Furthermore, the filter membrane in this embodiment is free of dead pores, solving the problem of dead pores in existing ceramic-sintered SPG membranes, which makes thorough cleaning and backwashing difficult.

[0057] Furthermore, the outer flow channels 212 between adjacent filter membranes 211 form directional fluid channels, which, together with the micropores 214, enable a more uniform transmembrane pressure distribution, avoiding localized eddies or dead zones. The inner flow channels 213 and outer flow channels 212, through the micropores 214, form controllable cross-flow shear forces, which is beneficial for generating microspheres with better dispersion. The parallel modular design allows for flexible increases or decreases in the number of filter membranes 211, satisfying both small-scale process optimization and scaling up to large-scale production. Filter membranes 211 can be maintained or replaced individually, reducing overall downtime losses due to localized blockage or damage. The collaborative work of multiple filter membranes 211 maintains more stable transmembrane pressure, and combined with the uniformity of the micropore size 214, ensures uniform microsphere particle size.

[0058] Optionally, adjacent filter membranes 211 are arranged at intervals. The interval arrangement of filter membranes 211 can reduce vibration interference and avoid the risk of mechanical damage to filter membranes 211 caused by dense arrangement.

[0059] Furthermore, the micropores 214 on the filter membrane 211 can be formed by laser processing. The micropores 214 formed by laser processing have a uniform pore distribution, which improves the uniformity of emulsification and solves the problem of random pore distribution and limited emulsification uniformity in existing SPG membranes formed by ceramic sintering.

[0060] Preferably, the micropores 214 on the filter membrane 211 are formed using a reflective Bezier beam processing method. In the prior art, micropores are typically formed by ceramic sintering, resulting in randomly distributed channels. This limits the emulsification uniformity of the membrane emulsification device. Furthermore, because random channels are prone to dead pores, thorough cleaning and backflushing are difficult, posing challenges for use in GMP (cleanroom) facilities. In this embodiment, the micropores 214 on the filter membrane 211 are preferably formed using a reflective Bezier beam processing method, which avoids dead pores and provides better pore size uniformity for the micropores 214.

[0061] It should be noted that reflective Bessel beams can be generated by a filter membrane processing system.

[0062] Optionally, the micropores 214 on the filter membrane 211 can be made of... Figure 7 The filter membrane processing system shown is used for processing. The structure and working principle of the filter membrane processing system of the present invention will be described in detail below.

[0063] In the late 1980s, Durnin of the University of Rochester formally proposed the concept of a diffraction-free beam. He essentially discovered a set of rigorous solutions to the zeroth-order Bessel function form of Maxwell's wave equation and experimentally proved, using simple optical components, that the corresponding wave of this particular solution is a Bessel beam, exhibiting diffraction-free characteristics. Due to the excellent optical propagation properties of diffraction-free Bessel beams, their research quickly attracted widespread attention from research groups both domestically and internationally.

[0064] The wave equation for an ideal Bessel beam is given by formula (1): Formula (1).

[0065] In formula (1), t represents electric field intensity; r represents spatial position coordinates; t represents time; c is the speed of light in vacuum. For the second-order partial derivative with respect to time; It is the Laplace operator.

[0066] A particular solution along the Z-axis can be expressed as formula (2): In formula (2), ε represents the electric field strength; r represents the spatial coordinates; t represents time; exp is the natural exponential function; i is the imaginary unit; For the longitudinal component of the propagation constant; ω is the angular frequency; z is the spatial coordinate along the main propagation direction of the beam (i.e., the Z-axis); For the transverse component of the propagation constant; The azimuth angle is x; x and y are rectangular coordinates in a plane perpendicular to the beam propagation direction (i.e., the Z-axis). Radial coordinates; This is a Bessel function.

[0067] For an ideal Bessel beam, its cross-sectional intensity distribution A Bessel beam is characterized by a central spot (main lobe) and numerous concentric rings (side lobes). The energy density of the main lobe is much higher than that of the side lobes, and the light intensity decreases sequentially from the inside out. However, the energy carried by the main lobe is equal to that of the side lobes, and the intensity distribution does not change with increasing propagation distance. The intensity of a Bessel beam does not change with propagation distance; this is commonly referred to as its "diffraction-free characteristic." Since the laser beam emitted from a laser in a real optical system is limited by an aperture, its beam width and energy are finite. In experiments, only an approximate Bessel beam can be obtained; that is, its "diffraction-free characteristic" manifests in practice as a limited distance along the propagation direction. Within this range, the lateral light intensity distribution remains essentially constant. Once this maximum distance is exceeded, the beam diverges and loses its "non-diffraction characteristic".

[0068] like Figure 10 These are simulation diagrams of the transverse and longitudinal light intensity distribution of Bessel and Gaussian beams: (a) and (b) are simulation diagrams of the light field of the Bessel beam; (c) and (d) are simulation diagrams of the light field of the Gaussian beam.

[0069] Figure 6 This is a schematic diagram of a filter film processing system based on a traditional Bessel beam. The laser source emits a laser beam, which, after passing through a beam expander, is incident on a transmission axial pyramid. The transmission axial pyramid transmits the incident Gaussian beam and converts it into a Bessel beam. This Bessel beam is then focused onto the processing station by a lens to drill holes in the workpiece. However, this transmission axial pyramid is not suitable for high-power laser drilling requirements.

[0070] like Figure 7 As shown in the figure, a specific embodiment of the present invention provides a filter membrane processing system. The filter membrane processing system includes a beam shaping component 110 and a transmission component 120; the beam shaping component 110 is used to reflect the incident laser and convert it into a Bessel beam; the transmission component 120 is disposed in the optical path of the Bessel beam and is used to transmit the non-diffraction region of the Bessel beam to the processing station.

[0071] In this embodiment, the incident laser beam is reflected and converted into a Bessel beam by the beam shaping component 110, instead of being transmitted to form a Bessel beam. Then, the non-diffraction region of the Bessel beam is transmitted to the processing station by the transmission component 120, allowing drilling of the workpiece placed at the processing station. The reflective design avoids energy absorption by the transmission element, making it suitable for long-term high-power processing. The reflective design does not require consideration of the material's transmittance, supporting incident lasers from the ultraviolet to the infrared band. The reflective design eliminates the thermal lens 121 effect, resulting in higher focal depth stability in the non-diffraction region of the Bessel beam, and also avoids the aperture inconsistency problem caused by heat accumulation in the transmission method.

[0072] Furthermore, the incident laser is a pulsed laser.

[0073] Furthermore, the beam shaping assembly 110 includes a reflective axial pyramid; the reflective axial pyramid is positioned in the optical path of the incident laser to reflect the incident laser and convert it into a Bessel beam. The reflective design avoids the dispersion problems of the transmitting material and is suitable for multi-wavelength / ultrafast lasers. The metal reflective film of the reflective axial pyramid (such as a gold film with an infrared reflectivity >98%) can withstand kilowatt-level lasers without thermal lensing effects. The reflection angle allows for a foldable optical path, saving space and making it suitable for integrated equipment.

[0074] As Figure 9 The images shown, including the incident laser after passing through the reflective axial pyramid and the spot image at the machining station, demonstrate that the reflective axial pyramid can convert the incident laser into a Bessel beam, and the transmission component can transmit the Bessel beam to the machining station.

[0075] like Figure 8 As shown, the base angle α of the reflective axial pyramid is further ranging from 0.5° to 15°. This design allows for flexible adaptation to different precision machining requirements while avoiding the limitations of traditional transmission-type axial pyramids. For example, Preferably, the base angle α of the reflective axial pyramid is 2° to 5°, which is suitable for long focal depths and wide-range processing.

[0076] like Figure 8 As shown, furthermore, the angle γ between the incident laser and the normal of the reflecting axial pyramid is half the base angle α. This further ensures the quality of the Bessel beam formed after passing through the reflecting axial pyramid.

[0077] Furthermore, the focal depth of the non-diffraction region is greater than the thickness of the filter membrane tube wall, ensuring that the non-diffraction region can cover the filter membrane tube wall, and micropores that penetrate the filter membrane tube wall can be punched on the filter membrane.

[0078] like Figure 8 As shown, after passing through the reflective axial pyramid, the focal depth of the Bessel beam is... The focal spot diameter of the Bessel beam is... ,in, Let be the focal radius of the Bessel beam.

[0079] in, The diffraction angle in the Bessel region can also be described as follows: The angle between the Bessel region and the optical axis of the reflected beam is π; π is 3.1415926. Represents the radius of the incident laser beam; The focal depth is the non-diffraction region of the Bessel beam.

[0080] For example, if the actual diameter of the emitted Bessel spot is 100 micrometers, but the required spot diameter for processing is 20 micrometers, then the focal length ratio of the field lens to the lens is 1:5.

[0081] In some embodiments, the filter membrane processing system further includes a galvanometer assembly 130; the galvanometer assembly 130 is disposed in the optical path of the Bessel beam and is used to adjust the deflection direction of the Bessel beam. By setting the galvanometer assembly 130, the deflection of the Bessel beam can be controlled, enabling rapid movement of the light spot on the workpiece. The operating speed of the galvanometer can generally reach 10 m / s, for example, the ExtraScan10 galvanometer.

[0082] Furthermore, the transfer assembly 120 includes a lens 121 and a field lens 122; the lens 121 is disposed at the incident end of the galvanometer assembly 130 and is used to focus the Bessel beam onto the galvanometer assembly 130; the field lens 122 is disposed at the exit end of the galvanometer assembly 130 and forms a 4F system with the lens 121, so that the field lens 122 transfers the non-diffraction region of the Bessel beam to the processing station.

[0083] In this embodiment, lens 121 and field lens 122 follow a 4F system to ensure that the diffraction-free characteristics of the Bessel beam are not compromised during scanning; wavefront distortion caused by traditional field lenses is avoided; and the depth of focus retention in the diffraction-free region is higher in this embodiment compared to non-4F systems. The galvanometer is placed on the central image plane of the 4F system, and its deflection only changes the beam angle rather than the focusing position, achieving zero field distortion and dynamic processing consistency.

[0084] Optionally, lens 121 is positioned at a distance from the optical center of the Bessel beam reflected and converged by beam shaping assembly 110, equal to the focal length of lens 121. In other words, the optical center of lens 121 must coincide with the optical axis of the Bessel beam, and the distance between lens 121 and the reflective axial pyramid must be equal to the focal length of lens 121. This allows the non-diffraction region of the Bessel beam to be effectively transferred to the processing station.

[0085] Furthermore, the filter membrane processing system also includes a beam expander 140; the beam expander 140 is disposed in the optical path of the incident laser and is used to adjust the beam size and / or divergence angle of the incident laser. Specifically, the beam expander 140 is disposed at the incident end of the reflective axial pyramid, and the incident laser passes through the beam expander 140 and is incident on the reflective axial pyramid; the reflective axial pyramid is used to reflect the incident laser and convert it into a Bessel beam.

[0086] Optionally, the beam expander 140 can be a 1x to 8x beam expander 140.

[0087] Furthermore, the filter membrane processing system also includes a laser source 160; the laser source 160 is used to emit incident laser light; the wavelength of the incident laser light... satisfy: In other words, the incident laser wavelength of the filter membrane processing system in this embodiment covers a broad band from deep ultraviolet (DUV) to terahertz (THz).

[0088] Optionally, the laser source 160 includes, but is not limited to, a picosecond laser.

[0089] Furthermore, the filter membrane processing system also includes a reflector 170; the reflector 170 is disposed at the exit end of the beam expander 140 and is used to reflect the beam emitted from the beam expander 140 to the reflective axial pyramid. By setting the reflector 170, the direction of the incident laser can be changed, making the layout of the entire system more flexible.

[0090] Furthermore, the filter membrane processing system also includes a polarization component 150; the polarization component 150 is positioned between the beam expander 140 and the laser source 160; the incident laser passes through the polarization component 150 and is directed towards the beam expander 140. This design can further optimize the polarization state of the incident laser to improve system efficiency and energy distribution; it also allows control of the shape of the filter membrane perforations by preset polarization direction. The polarization component 150 can block back-reflected light (such as laser light reflected from the processing station) from returning to the laser source 160, preventing instability or damage to the light source.

[0091] Optionally, the polarization assembly 150 includes a polarizer 152 and a half-wave plate 151; the half-wave plate 151 is disposed between the laser source 160 and the polarizer 152.

[0092] It should be noted that the material of the filter membrane is not limited in the specific embodiments of the present invention. Optionally, the filter membrane can be made of metal. Metals include, but are not limited to, stainless steel, copper, and aluminum. Figure 11 The filter membrane processing system of this embodiment is used to drill 1-micron pores in stainless steel.

[0093] A specific embodiment of the present invention provides a filter membrane processing method. This filter membrane processing method employs the filter membrane processing system described in any of the above embodiments. The filter membrane processing method includes: S100. Place the workpiece to be processed in the processing station of the filter membrane processing system.

[0094] S200, the incident laser is emitted into the beam shaping assembly 110, and the beam shaping assembly 110 reflects the incident laser and converts it into a Bessel beam.

[0095] Specifically, the laser source 160 is activated to emit an incident laser. The incident laser passes through a half-wave plate 151, a polarizer 152, a beam expander 140, and a reflector 170 before being incident on a reflective axial pyramid. The reflective axial pyramid reflects the incident laser and converts it into a Bessel beam.

[0096] S300 and the transfer component 120 transfer the non-diffraction region of the Bessel beam to the processing station to process micropores on the workpiece to obtain a filter membrane.

[0097] Specifically, the Bessel beam is focused by lens 121 onto galvanometer assembly 130; the Bessel beam emitted from galvanometer assembly 130 is focused by field lens 122 to transmit the non-diffraction region of the Bessel beam to the processing station, thereby realizing the drilling of the workpiece to be processed; the deflection of the Bessel beam is adjusted by galvanometer assembly 130 to achieve dynamic drilling, and finally the filter membrane is obtained.

[0098] Furthermore, the pore size of the micropore 214 ranges from 0.1 micrometers to 40 micrometers. In other words, the pore size of the micropore 214 can be 0.1 micrometers, 40 micrometers, or any value between 0.1 micrometers and 40 micrometers.

[0099] like Figure 2 As shown, the membrane emulsification device 210 further includes a housing 215; the housing 215 has a receiving cavity inside; multiple filter membranes 211 are arranged in parallel in the receiving cavity; and an outer flow channel 212 is located in the receiving cavity. The housing 215 has a dispersed phase inlet, an outer aqueous phase inlet, and an outer aqueous phase outlet; the dispersed phase inlet is connected to the outer flow channel 212, the outer aqueous phase inlet is connected to one end of the inner flow channel 213, and the outer aqueous phase outlet is connected to the other end of the inner flow channel 213.

[0100] In this embodiment, the receiving cavity provides installation space for the filter membrane 211, and the outer shell 215 isolates the filter membrane 211 from the outside world to prevent environmental particles or microorganisms from contaminating the microsphere products.

[0101] Optionally, multiple filter membranes 211 are arranged in a periodic array within the receiving cavity.

[0102] Optionally, the outer casing 215 is also provided with a vent for venting air; the vent is connected to the outer flow channel 212. When the dispersed phase is injected into the outer flow channel 212, the vent can be opened to vent the air in the outer flow channel 212 and the inner flow channel 213.

[0103] In some embodiments, the preparation system for microbial and nucleic acid removal materials based on high-temperature stable sustained-release microspheres further includes an emulsion storage device 240; the emulsion storage device 240 is connected to an inner flow channel 213 and is used to store the emulsion discharged from the inner flow channel 213. Specifically, an external aqueous phase outlet is connected to the emulsion storage device 240 and is used to discharge the emulsion from the inner flow channel 213 into the emulsion storage device 240 for storage.

[0104] In this embodiment, the external aqueous phase outlet is directly connected to the emulsion storage device 240 (such as a buffer tank with stirring) to achieve immediate collection and stable storage of the emulsion and avoid droplet aggregation.

[0105] Furthermore, the emulsion storage device 240 includes a third storage tank and a third agitator; the third storage tank is connected to the inner flow channel 213 and is used to store the emulsion. The third agitator is installed in the third storage tank to reduce the risk of emulsion droplet aggregation in the emulsion.

[0106] In some embodiments, the preparation system of microbial and nucleic acid removal materials based on high-temperature stable sustained-release microspheres further includes a pressure supply device 250; the pressure supply device 250 is connected to the outer channel 212 and is used to introduce protective gas into the outer channel 212 to push the dispersed phase through the micropores 214 to form droplets in the inner channel 213.

[0107] In this embodiment, by setting up a pressure supply device 250, the speed at which the dispersed phase (such as the oil phase) permeates through the micropores 214 can be controlled by adjusting the gas pressure (such as nitrogen or air), thereby achieving dynamic control of droplet formation. Compared to mechanical pumping, gas pressure drive is more stable and avoids uneven droplet size caused by pulsed flow. The gas forms an "air cushion" barrier in the outer flow channel 212, reducing direct contact between the two phases and preventing component mixing (such as surfactant migration). Gas-assisted propulsion can reduce the retention of high-viscosity dispersed phase in the micropores 214, reducing the probability of clogging.

[0108] Furthermore, the pressure supply device 250 includes a gas tank (not shown in the figure), an air pump 251, and a pressure regulator 252. The gas tank stores protective gas. The inlet of the air pump 251 is connected to the outlet of the gas tank, and the outlet of the air pump 251 is connected to the outer flow channel 212 for supplying protective gas to the outer flow channel 212. The pressure regulator 252 is located at the outlet of the air pump 251 and is used to adjust the gas pressure entering the outer flow channel 212. The gas pressure entering the outer flow channel 212 can be adjusted by adjusting the pressure regulator 252 according to the viscosity of the dispersed phase and the target particle size of the microspheres to prepare microspheres that meet the target particle size.

[0109] Optional, the protective gas includes, but is not limited to, nitrogen.

[0110] Furthermore, the pressure supply device 250 also includes a sixth three-way valve 254 and a third three-way valve 253; the inlet of the sixth three-way valve 254 is connected to the outlet of the air pump 251, and the first outlet of the sixth three-way valve 254 is connected to the outer flow channel 212; the second outlet of the sixth three-way valve 254 is connected to the inlet of the third three-way valve 253, the first outlet of the third three-way valve 253 is connected to the inlet of the first dispersed phase storage unit 221, and the second outlet of the third three-way valve 253 is connected to the inlet of the second dispersed phase storage unit 222. When it is necessary to inject the dispersed phase of the first dispersed phase storage unit 221 into the outer flow channel 212, the gas discharged by the air pump 251 can enter the inlet of the third three-way valve 253 through the second outlet of the sixth three-way valve 254, and enter the first dispersed phase storage unit 221 from the first outlet of the third three-way valve 253, so as to force the dispersed phase into the outer flow channel 212. When it is necessary to inject the dispersed phase from the second dispersed phase storage unit 222 into the outer flow channel 212, the gas discharged by the air pump 251 can enter the inlet of the third three-way valve 253 through the second outlet of the sixth three-way valve 254, and then enter the second dispersed phase storage unit 222 from the second outlet of the third three-way valve 253, so as to force the dispersed phase into the outer flow channel 212. When it is necessary to pressurize the outer flow channel 212, the protective gas discharged by the air pump 251 is discharged into the outer flow channel 212 through the first outlet of the sixth three-way valve 254.

[0111] In some embodiments, the preparation system of microbial and nucleic acid removal materials based on high-temperature stable slow-release microspheres further includes a dispersed phase supply device 220 and an external aqueous phase supply device 230; the dispersed phase supply device 220 is connected to the external flow channel 212 and is used to inject the dispersed phase into the external flow channel 212; the external aqueous phase supply device 230 is connected to the internal flow channel 213 to form an external aqueous phase circulation loop.

[0112] In this embodiment, the flow pattern of the dispersed phase in the outer channel 212 and the outer aqueous phase in the inner channel 213 enhances the turbulence effect, reduces the risk of micropore 214 clogging, and increases flux. Furthermore, the two phases mix rapidly near the inner surface of the filter membrane 211, avoiding pre-emulsification and reducing batch variations caused by phase separation.

[0113] Furthermore, the dispersed phase supply device 220 includes a dispersed phase storage module; the dispersed phase storage module includes a first dispersed phase storage unit 221, a second dispersed phase storage unit 222, and a first valve body unit 223; both the first dispersed phase storage unit 221 and the second dispersed phase storage unit 222 are used to store dispersed phase; the first valve body unit 223 has a first conducting state and a second conducting state; in the first conducting state, the first dispersed phase storage unit 221 injects dispersed phase into the outer flow channel 212; in the second conducting state, the second dispersed phase storage unit 222 injects dispersed phase into the outer flow channel 212. This design ensures continuous production of the system. For example, after the dispersed phase stored in the first dispersed phase storage unit 221 is used up, the first valve body unit 223 can be switched from the first conducting state to the second conducting state, so that the dispersed phase in the second dispersed phase storage unit 222 is injected into the outer flow channel 212, thereby ensuring the continuity of production.

[0114] Furthermore, the first dispersed phase storage unit 221 includes a first storage tank and a first stirrer; the first stirrer is installed inside the first storage tank, which contains the dispersed phase. By providing the first stirrer, the dispersiond phase can be prevented from accumulating inside the first storage tank.

[0115] Optionally, the first dispersed phase storage unit 221 and the second dispersed phase storage unit 222 may have the same structure.

[0116] It should be noted that, in this embodiment, there is no limitation on the number of the first dispersed phase storage unit 221 and the second dispersed phase storage unit 222.

[0117] Furthermore, the first valve body unit 223 includes a first three-way valve; the outer flow channel 212 is connected to the first dispersed phase storage unit 221 and the second dispersed phase storage unit 222 respectively through the first three-way valve. Specifically, the first inlet of the first three-way valve is connected to the outlet of the first dispersed phase storage unit 221, the second inlet of the first three-way valve is connected to the outlet of the second dispersed phase storage unit 222, and the outlet of the first three-way valve is connected to the outer flow channel 212 through the dispersion inlet.

[0118] Preferably, the first three-way valve is an electromagnetic three-way valve, which facilitates automated control.

[0119] Furthermore, the external aqueous phase supply device 230 includes an external aqueous phase storage module 231 and a circulation power source 232. The external aqueous phase storage module 231 is used to store the external aqueous phase. The inlet of the external aqueous phase storage module 231 is connected to the outlet of the inner flow channel 213, and the outlet of the external aqueous phase supply device 230 is connected to the inlet of the inner flow channel 213 to form an external aqueous phase circulation loop. The circulation power source 232 is located in the external aqueous phase circulation loop. When it is necessary to inject the external aqueous phase into the inner flow channel 213, the circulation power source 232 is activated, and the external aqueous phase in the external aqueous phase storage module 231 enters the inner flow channel 213. The external aqueous phase injected into the inner flow channel 213 washes the inner surface of the filter membrane 211, causing the emulsion droplets to peel off from the micropores 214 and disperse into the external aqueous phase, and finally return to the external aqueous phase storage module 231. After the emulsification process is completed, the emulsion in the inner flow channel 213 can be discharged into the emulsion storage device 240 for storage.

[0120] Furthermore, the external aqueous phase storage module 231 includes a first external aqueous phase storage unit 2311, a second external aqueous phase storage unit 2312, and a second valve body unit. Both the first and second external aqueous phase storage units 2311 and 2312 are used to store external aqueous phase. The second valve body unit has a third open state and a fourth open state. In the third open state, the first external aqueous phase storage unit 2311 injects external aqueous phase into the inner flow channel 213; in the fourth open state, the second external aqueous phase storage unit 2312 injects external aqueous phase into the inner flow channel 213. This design ensures continuous production of the system. For example, after the external aqueous phase stored in the first external aqueous phase storage unit 2311 is used up, the second valve body unit can be switched from the third open state to the fourth open state, allowing the external aqueous phase in the second external aqueous phase storage unit 2312 to be injected into the inner flow channel 213, thus ensuring continuous production.

[0121] Optionally, the second external aqueous phase storage unit 2312 includes a second storage tank and a second stirrer; the second stirrer is installed inside the second storage tank, which contains the external aqueous phase. By providing the second stirrer, the accumulation of emulsion droplets in the second storage tank can be prevented.

[0122] Optionally, the first external aqueous phase storage unit 2311 and the second external aqueous phase storage unit 2312 may have the same structure.

[0123] Optionally, the second valve body unit includes a second three-way valve 2313 and a fourth three-way valve 2314; the inlet of the inner flow channel 213 is connected to the outlet of the first external water phase storage unit 2311 and the outlet of the second external water phase storage unit 2312 respectively through the second three-way valve 2313; the outlet of the inner flow channel 213 is connected to the inlet of the first external water phase storage unit 2311 and the inlet of the second external water phase storage unit 2312 respectively through the fourth three-way valve 2314. Specifically, the first inlet and outlet of the second three-way valve 2313 are connected to the outlet of the first external water phase storage unit 2311, the second inlet of the second three-way valve 2313 is connected to the outlet of the second external water phase storage unit 2312, and the outlet of the second three-way valve 2313 is connected to the inlet of the inner flow channel 213 through the circulating power source 232. The first outlet of the fourth three-way valve 2314 is connected to the inlet of the first external water phase storage unit 2311, the second outlet of the second three-way valve 2313 is connected to the inlet of the second external water phase storage unit 2312, and the inlet of the second three-way valve 2313 is connected to the outlet of the internal flow channel 213.

[0124] Preferably, the second three-way valve 2313 is an electromagnetic three-way valve, which facilitates automated control.

[0125] Preferably, the fourth three-way valve 2314 is an electromagnetic three-way valve, which facilitates automated control.

[0126] Furthermore, the circulating power source 232 includes a circulating pump 2321 and a flow detection unit 2322; the flow detection unit 2322 is located at the outlet of the circulating pump 2321 and is used to detect the flow rate of the external water phase.

[0127] Optionally, the flow detection unit 2322 includes a flow meter.

[0128] In some embodiments, the microbial and nucleic acid removal material preparation system based on high-temperature stable sustained-release microspheres further includes a third valve body unit 260; the emulsion storage device 240 is connected to the outlet of the inner flow channel 213; the third valve body unit 260 has a fifth conducting state and a sixth conducting state; in the fifth conducting state, the external aqueous phase supply device 230 is connected to the inner flow channel 213 to form an external aqueous phase circulation loop; in the sixth conducting state, the inlet of the inner flow channel 213 is connected to the emulsion storage device 240 for discharging the emulsion.

[0129] Specifically, the third valve body unit 260 includes a fifth three-way valve; the inlet of the fifth three-way valve is connected to the outlet of the inner flow channel 213, the first outlet of the fifth three-way valve is connected to the emulsion storage device 240, and the second outlet of the fifth three-way valve is connected to the inlet of the fourth three-way valve 2314.

[0130] Optionally, the fifth three-way valve can be a solenoid three-way valve for easy automated control.

[0131] like Figure 5 As shown, a specific embodiment of the second aspect of the present invention provides a method for preparing microbial and nucleic acid scavenging materials based on high-temperature stable sustained-release microspheres, comprising the following steps: S00: The first surfactant is mixed with water to obtain the outer aqueous phase; the aqueous phase raw material is mixed with the second surfactant to obtain the inner aqueous phase; the oil phase raw material is dissolved in an organic solvent to obtain an oil phase solution; then the inner aqueous phase and the oil phase solution are mixed, and the water-in-oil emulsion obtained by ultrasonication is the dispersed phase.

[0132] S10: Inject the dispersed phase into the outer channel 212 and inject the external aqueous phase into the inner channel 213.

[0133] Specifically, the dispersed phase in the dispersed phase storage module is circulated into the outer flow channel 212 to fill the outer flow channel 212; the circulation power source 232 is started to circulate the outer water phase in the outer water phase storage module 231 into the inner flow channel 213.

[0134] S20: A protective gas is introduced into the outer channel 212, which pushes the dispersed phase through the micropores 214 to form droplets in the inner channel 213, and mixes with the outer aqueous phase to form an emulsion.

[0135] Specifically, when the pressure supply device 250 is turned on, the protective gas enters the outer flow channel 212. The dispersed phase will pass through the micropores 214 under the push of the high-pressure gas, form droplets in the inner flow channel 213, and disperse into the outer aqueous phase under the flushing of the outer aqueous phase to form an emulsion.

[0136] S30: After emulsification is completed, the emulsion in the inner channel 213 is discharged into the emulsion storage device 240 for storage.

[0137] Specifically, after emulsification is completed, the circulating power source 232 is stopped, the conduction state of the third valve body unit 260 is switched, and the emulsion in the inner flow channel 213 is discharged into the emulsion storage device 240 for storage.

[0138] S40: The emulsion is stirred, the solvent is evaporated and freeze-dried, and then high-temperature complexation is carried out at 80℃~100℃.

[0139] To further illustrate the technical solution of the present invention, specific embodiments are provided below: The following embodiments use the above-described preparation system. Specifically, the pore size of the micropore 214 is 1 micrometer, and the base angle α of the reflective axial pyramid is 2°.

[0140] Example 1 This embodiment provides a microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres, which is prepared from oil-phase raw materials and aqueous-phase raw materials; wherein, the oil-phase raw material is poly-L-lactic acid with a molecular weight of 50,000; the aqueous-phase raw materials are polyethyleneimine (molecular weight of 3,000), polyhexamethylene biguanide and benzalkonium chloride in a mass ratio of 1:1:2; the volume ratio of oil-phase raw materials to aqueous-phase raw materials is 1:3.

[0141] The preparation method of the microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres includes the following steps: S1: Hexadecyltrimethylammonium bromide is mixed with water to obtain an external aqueous phase with a surfactant concentration of 1% (w / v); the aqueous phase raw material is mixed with hexadecyltrimethylammonium bromide to obtain an internal aqueous phase with a surfactant concentration of 1% (w / v); the oil phase raw material is dissolved in dichloromethane to obtain an oil phase solution with an oil phase raw material concentration of 10 wt%; then the internal aqueous phase and the oil phase solution are mixed at a mass ratio of 1:9, and the water-in-oil emulsion obtained by probe ultrasound is the dispersed phase; S2: The air pump delivers protective gas into the first dispersed phase storage unit of the dispersed phase supply device, injecting the dispersed phase in the first dispersed phase storage unit into the outer channel of the membrane emulsification device, filling the outer channel with dispersed phase; the circulation power source is started, and the outer aqueous phase stored in the second outer aqueous phase storage unit is pumped into the inner channel; forming an outer aqueous phase circulation loop. By adjusting the conduction state of the sixth three-way valve, the gas path is switched, allowing protective gas to enter the outer channel to increase the pressure in the outer channel to 0.05MPa, causing the dispersed phase to pass through the micropores to form emulsion droplets. The outer aqueous phase in the inner channel flushes and disperses the emulsion droplets into the outer aqueous phase to form an emulsion. S3: After emulsification, the emulsion in the inner channel is dried, and then the dried microspheres are subjected to high-temperature complexation at 90°C for 60 minutes to obtain microbial and nucleic acid removal materials based on high-temperature stable slow-release microspheres.

[0142] like Figure 12 As shown, the particle size of the microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres is 2.1µm±0.37µm.

[0143] Example 2 This embodiment provides a microbial and nucleic acid scavenging material based on high-temperature stable sustained-release microspheres. The only difference between this embodiment and Example 1 is that the internal aqueous phase raw materials include polyethyleneimine, polyhexamethylene biguanide, and benzalkonium chloride in a mass ratio of 1:4:4. The resulting microbial and nucleic acid scavenging material based on high-temperature stable sustained-release microspheres has a particle size of 2.2µm ± 0.43µm.

[0144] Example 3 This embodiment provides a microbial and nucleic acid scavenging material based on high-temperature stable sustained-release microspheres, which differs from Example 1 only in that the volume ratio of the internal aqueous phase raw material to the oil phase raw material is 1:4. The particle size of the obtained microbial and nucleic acid scavenging material based on high-temperature stable sustained-release microspheres is 2.6µm ± 0.64µm.

[0145] Example 4 This embodiment provides a microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres. The difference between this embodiment and Embodiment 1 is that polyethyleneimine with a molecular weight of 3000 is replaced by polyethyleneimine with a molecular weight of 18000 in equal amounts.

[0146] The particle size of the obtained microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres was 2.2µm±0.52µm.

[0147] Example 5 This embodiment provides a microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres, which differs from Embodiment 1 only in that: polyethyleneimine is replaced with chitosan in equal amounts.

[0148] The particle size of the obtained microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres was 2.3µm±0.46µm.

[0149] Example 6 This embodiment provides a microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres. The only difference between this material and Example 1 is that the mass ratio of polyhexamethylene biguanide to polyethyleneimine is 4:1.

[0150] Example 7 This embodiment provides a microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres. The only difference between this material and Example 1 is that its preparation method does not include a high-temperature complexation step.

[0151] Comparative Example 1 This comparative example provides a microbial and nucleic acid scavenging material based on high-temperature stable sustained-release microspheres. The difference between this and Example 1 is that the preparation method of the high-temperature stable sustained-release microsphere-based microbial and nucleic acid scavenging material differs from Example 1 only in that poly-L-lactic acid is replaced with an equal amount of polylactic-co-glycolic acid (PLGA). The final microsphere particle size is 2.3µm ± 0.47µm.

[0152] Comparative Example 2 This comparative example provides a microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres. The difference between this and Example 1 is that the polyethyleneimine in the aqueous phase raw material is replaced with an equal amount of polyhexamethylene biguanide. The resulting microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres has a particle size of 2.2 µm ± 0.51 µm.

[0153] Comparative Example 3 This comparative example provides a microbial and nucleic acid scavenging material based on high-temperature stable sustained-release microspheres. The difference between this material and Example 1 is that poly-L-lactic acid is replaced in equal amounts with hydrogenated lecithin. The resulting microbial and nucleic acid scavenging material based on high-temperature stable sustained-release microspheres has a particle size of 3.6 ± 0.68 µm.

[0154] Test case This invention verifies the bactericidal effect, long-lasting effect, and high-temperature stability of the microbial and nucleic acid removal materials based on high-temperature stable sustained-release microspheres prepared in the above embodiments and comparative examples.

[0155] 1. Instant sterilization effect after high-temperature treatment Test method: The microbial and nucleic acid removal materials based on high-temperature stable slow-release microspheres prepared in the examples and comparative examples were formulated into a 0.002 wt% disinfectant solution using ultrapure water. The solution was then pretreated at 95°C for one hour to simulate a high-temperature scenario, and after returning to room temperature, the following experiments were conducted: 1. Take 100 μL of E. coli (10 μL) 6 The CFU suspension was added dropwise perpendicular to the center of the glass support, and the filter paper was held by tweezers to absorb and spread the film. The film was dried at room temperature for 15 minutes to form a uniform film. 2. Using a calibrated spray bottle (output 0.8 mL / s), spray the pretreated disinfectant solution at a uniform speed in a Z-shaped trajectory from a distance of 30 cm from the surface. Use 1 mL and let it stand until the specified time point.

[0156] 3. Three sampling areas were selected using the nine-square grid method, and samples were taken at 1 and 5 minutes respectively. After sampling, the samples were placed in a neutralizing agent (1L PBS plus 1g sodium thiosulfate + 10g Tween 80 + 5g lecithin). 4. Then centrifuge at 6000 rpm for 5 min, resuspend in 100 μL LB medium, spread on solid culture medium, and incubate overnight. Take photos and count the samples for analysis.

[0157] Test results are available Figure 13The results showed that the extremely low concentration (0.002 wt%) of the high-temperature stable sustained-release microsphere-based microbial and nucleic acid removal material in Example 1 could completely kill Escherichia coli within 1 minute at high temperature, demonstrating excellent bactericidal performance. Further comparative experiments showed that the high-temperature bactericidal effect of Examples 2-4 was comparable to that of Example 1, also capable of efficiently killing Escherichia coli in a short time. However, when the cationic polymer in Example 1 was replaced (Example 5), or a formulation outside the preferred formulation range of this invention was used (Example 6), or the high-temperature complexation step was omitted (Example 7), the disinfection effect decreased, failing to reach the high-efficiency killing level of Example 1. This indicates that the specific formulation and process conditions used in Example 1 of this invention are crucial for achieving the high-efficiency disinfection performance of the high-temperature stable sustained-release microsphere-based microbial and nucleic acid removal material, and are key to achieving rapid and thorough killing of Escherichia coli. Comparative Example 1 showed no disinfection effect at all. The high-temperature bactericidal effect of the high-temperature stable sustained-release microsphere-based microbial and nucleic acid removal materials prepared under the formulations of Comparative Examples 2-3 was significantly worse than that of the examples.

[0158] 2. Long-lasting sterilization performance at high temperatures Test method: The microbial and nucleic acid removal materials based on high-temperature stable sustained-release microspheres prepared in the examples and comparative examples were formulated into a 0.002 wt% disinfectant solution using ultrapure water and pretreated at 95°C for one hour. The following experiments were then conducted: 1. Using a calibrated spray bottle (output 0.8 mL / s), spray the pretreated disinfectant solution onto the stainless steel plate surface at a uniform speed in a Z-shaped trajectory from a distance of 30 cm away from the surface. Use 1 mL of the solution and let it stand at 60 degrees Celsius until the specified time point.

[0159] 2. 100 μL of E. coli (10⁶ CFU) was applied to stainless steel plates on days 7, 14, 21, and 28, respectively.

[0160] 3. Three sampling areas were selected using the nine-square grid method. Samples were taken at 5 minutes and then placed in a neutralizing agent (1L PBS with 1g sodium thiosulfate, 10g Tween 80, and 5g lecithin). 4. Then centrifuge at 6000 rpm for 5 min, resuspend in 100 μL LB medium, spread on solid culture medium, and incubate overnight. Take photos and count the samples for analysis.

[0161] Test results are available Figure 14Experimental results show that, under high-temperature conditions, the bactericidal effect of this disinfectant is consistent with the trend of the aforementioned instantaneous bactericidal effect: the microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres prepared in Example 1 can maintain a high-efficiency bactericidal effect under low concentration (0.002 wt%) conditions. Meanwhile, the long-term bactericidal effect of the microbial and nucleic acid removal materials based on high-temperature stable sustained-release microspheres in Examples 2-4 is comparable to that of Example 1. This characteristic indicates that the disinfectant has stable chemical properties and long-lasting bactericidal activity in high-temperature environments, effectively addressing microbial contamination problems in complex environments. The long-term bactericidal ability of Examples 5 (cationic polymer replacement), 6 (non-preferred formulation), and 7 (without high-temperature complexation step) is inferior to that of Example 1, further confirming the superiority and necessity of the preferred formulation and process of this invention. Similarly, Comparative Example 1 has no effect, and the long-term bactericidal effect of the microbial and nucleic acid removal materials based on high-temperature stable sustained-release microspheres prepared in Comparative Examples 2-3 is worse than that of Examples 5-7.

[0162] 3. Virus disinfection performance at high temperatures The microbial and nucleic acid removal materials based on high-temperature stable slow-release microspheres prepared in the examples and comparative examples were respectively prepared into 0.05wt% and 0.025wt% disinfectant solutions using ultrapure water, and then pretreated at 95°C for one hour. The following experiments were then conducted: 1. Take 1 ml of ASFV virus / H1S1 virus (10CT <) suspension and drop it vertically to the center of the carrier. Hold the filter paper edge with tweezers to adsorb and spread it. Dry at room temperature for 15 min to form a uniform film layer. 2. Using a calibration spray bottle (output 0.8 mL / s), spray the surface at a uniform speed in a Z-shaped trajectory from a distance of 30 cm, using 10 mL of the spray bottle, and let it stand until the specified time point.

[0163] 3. Three sampling areas were selected using the nine-square grid method, and samples were taken at 10, 20, and 30 minutes respectively. After sampling, the samples were placed in a neutralizing agent (1L PBS with 1g sodium thiosulfate + 10g Tween 80 + 5g lecithin). 4. Extract viral nucleic acid for RT-PCR reaction and count the CT value.

[0164] The test results are shown in Tables 1 and 2: Table 1. Disinfection efficacy against ASFV virus

[0165] Table 2. Disinfection effect of the high-temperature stable slow-release microsphere-based microbial and nucleic acid removal material prepared in Example 1 on H1S1 virus.

[0166] To further verify the broad-spectrum disinfection capability of the high-temperature stable slow-release microsphere-based microbial and nucleic acid removal material of this invention, the inventors conducted specific tests on its disinfection efficacy against African swine fever virus (ASFV) and H1N1 influenza virus under high-temperature conditions. The experimental results showed that the disinfection effect of this disinfectant under high-temperature conditions exhibited a consistent trend with previous test results against Escherichia coli. The microbial and nucleic acid removal materials based on high-temperature stable slow-release microspheres prepared in Examples 1-4 can rapidly destroy the structure of ASFV virus, effectively inhibit viral activity, and demonstrate strong disinfection capabilities. This disinfectant also performs excellently against H1N1 influenza virus, not only rapidly killing the H1N1 virus but also maintaining its inhibitory effect on the virus in subsequent tests, preventing further spread and infection.

[0167] Compared with other examples, although Examples 5 (cationic polymer replacement), 6 (non-preferred formulation), and 7 (no high-temperature complexation step) also showed a certain degree of sterilization effect under high-temperature conditions, they were slightly inferior to Examples 1-4. In Comparative Examples 1 and 3, after replacing poly-L-lactic acid with an equal amount of polylactic-co-glycolic acid (PLGA), the results showed that the microbial and nucleic acid removal materials based on high-temperature stable sustained-release microspheres obtained with the PLGA-containing formulation had a certain bactericidal and disinfection ability at room temperature, but at high temperatures, their thermal stability was poor, and their bactericidal and disinfection ability decreased significantly. The microbial and nucleic acid removal materials based on high-temperature stable sustained-release microspheres prepared in Comparative Example 2 showed a significant difference from the examples in both instantaneous killing ability and long-term inhibitory ability.

[0168] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres, characterized in that, The microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres is mainly prepared from an oil phase raw material, an inner aqueous phase raw material, and an outer aqueous phase; the oil phase raw material includes poly-L-lactic acid; the inner aqueous phase raw material is a mixture of cationic polymer and benzalkonium chloride; the cationic polymer includes any two or three of polyhexamethylene biguanide, polyethyleneimine, and chitosan.

2. The microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres according to claim 1, characterized in that, The cationic polymer is a mixture of polyhexamethylene biguanide and polyethyleneimine; Preferably, in the cationic polymer, the mass ratio of polyhexamethylene biguanide to polyethyleneimine is (1~4):(1~4).

3. The microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres according to claim 2, characterized in that, The content of polyethyleneimine in the aqueous phase raw material is 1wt%~25wt%.

4. The microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres according to any one of claims 1 to 3, characterized in that, The internal aqueous phase raw material is a mixture of cationic polymer and benzalkonium chloride in a mass ratio of (2~5):(2~4); And / or, the volume ratio of the oil phase feedstock to the internal aqueous phase feedstock is 1:(3~5).

5. The microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres according to any one of claims 1 to 3, characterized in that, The particle size of the microbial and nucleic acid removal material based on high-temperature stable slow-release microspheres is 1µm~20µm.

6. The method for preparing microbial and nucleic acid removal materials based on high-temperature stable sustained-release microspheres according to any one of claims 1 to 5, characterized in that, Microbial and nucleic acid removal materials based on high-temperature stable sustained-release microspheres are prepared using a microsphere preparation system. The microsphere preparation system includes a membrane emulsification device (210); the membrane emulsification device (210) includes multiple filter membranes (211) arranged in parallel; an outer flow channel (212) is formed between two adjacent filter membranes (211); an inner flow channel (213) is formed in the filter membrane (211) along its own axial direction; multiple micropores (214) are opened on the tube wall of the filter membrane (211); the outer flow channel (212) is connected to the inner flow channel (213) through the micropores (214); The preparation method includes the following steps: S1: The first surfactant is mixed with water to obtain the outer aqueous phase; the inner aqueous phase raw material is mixed with the second surfactant to obtain the inner aqueous phase; the oil phase raw material is dissolved in an organic solvent to obtain an oil phase solution; then the inner aqueous phase and the oil phase solution are mixed, and the water-in-oil emulsion obtained by ultrasonication is the dispersed phase; S2: Inject the dispersed phase into the outer channel (212) and inject the outer aqueous phase into the inner channel (213); introduce protective gas into the outer channel (212) to push the dispersed phase through the micropores (214) to form droplets in the inner channel (213) and mix with the outer aqueous phase to form an emulsion; S3: The emulsion is dried and then subjected to high-temperature complexation; preferably, the high-temperature complexation temperature is 80℃~100℃.

7. The method for preparing microbial and nucleic acid scavenging materials based on high-temperature stable sustained-release microspheres according to claim 6, characterized in that, The first surfactant and the second surfactant each independently, identically, or differently comprise polyvinyl alcohol and / or hexadecyltrimethylammonium bromide; the concentration of the first surfactant in the external aqueous phase is 0.5 wt% to 1.5 wt%; the concentration of the second surfactant in the internal aqueous phase is 0.5 wt% to 1.5 wt%. And / or, the organic solvent includes dichloromethane.

8. The method for preparing microbial and nucleic acid scavenging materials based on high-temperature stable sustained-release microspheres according to claim 6, characterized in that, The mass ratio of the internal aqueous phase to the oil phase solution is 1:(5~10).

9. The application of the microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres according to any one of claims 1 to 5, or the microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres prepared by the preparation method according to any one of claims 6 to 8, under high-temperature conditions; preferably, the temperature of the high-temperature conditions is 50 to 95°C.

10. A disinfection product, characterized in that, The product contains the microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres as described in any one of claims 1 to 5, or the microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres prepared by the preparation method described in any one of claims 6 to 8; preferably, the content of the microbial and nucleic acid removal material based on high-temperature stable sustained-release microspheres in the disinfection product is 0.001wt% to 0.01wt%.

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