A method, device and system for preparing multi-faceted anisotropic microspheres based on electrically assisted gas shearing

Abstract

The application discloses a method, device and system for preparing multifaceted anisotropic microspheres based on electric auxiliary gas shearing, and the system can be used for preparing microspheres by combining high-voltage electrostatic and gas shearing methods. The target microspheres still have a multifaceted anisotropic microsphere structure in the case that the particle diameter is less than 100 microns. The particle diameter of the microspheres is regulated by adjusting the high-voltage electrostatic voltage, airflow speed, solution pushing speed, coil diameter, distance between the solution receiving platform and the gas channel outlet, and the outlet arrangement mode of the gas channel and the solution channel. The experimental equipment is simple, safe and has rich expandability. The materials used are all biobased degradable materials. Based on these advantages, the small-particle-diameter anisotropic microspheres prepared by the method have very wide application scenarios.

Description

Technical Field

[0001] This invention belongs to the field of polymer technology, specifically relating to a method, apparatus, and system for preparing multifaceted anisotropic microspheres based on electric-assisted gas shearing. Background Technology

[0002] In recent years, anisotropic microspheres have attracted widespread attention due to their unique asymmetry, which gives them unique physical and chemical properties. Sodium alginate molecules are composed of β-D-mannuronic acid (M) and α-L-guluronic acid (G) linked by (1→4) bonds. Due to their good biocompatibility and biosafety, they are widely used in food, medicine and other fields.

[0003] Multifaceted anisotropic materials can be applied in many fields, including constructing multi-drug delivery systems, serving as carriers for cell culture microenvironments, serving as carriers for multi-level enzyme-linked reactions, multi-target biological detection, and multifunctional coding materials.

[0004] Several novel methods have been successfully applied to the preparation of faceted anisotropic microspheres, commonly including microfluidics, coaxial electroinjection, and gas shearing. However, these methods have inherent drawbacks. For example, fluidic methods rely excessively on redundant components such as oil and surfactants, posing potential biosafety risks; coaxial electroinjection yields relatively low output; and gas shearing produces microspheres with excessively large particle sizes. These shortcomings limit the widespread application of faceted anisotropic microspheres in the biomedical field. Therefore, simple and environmentally friendly new strategies are urgently needed, and developing new methods for faceted anisotropic microspheres smaller than 100 μm remains a challenging task. Summary of the Invention

[0005] The purpose of this section is to outline some aspects of embodiments of the present invention and to briefly describe some preferred embodiments. Simplifications or omissions may be made in this section, as well as in the abstract and title of this application, to avoid obscuring the purpose of these documents; however, such simplifications or omissions should not be construed as limiting the scope of the invention.

[0006] In view of the problems existing in the above and / or prior art, the present invention is proposed.

[0007] Therefore, the purpose of this invention is to overcome the shortcomings of the prior art and provide a method for preparing multifaceted anisotropic microspheres based on electrically assisted gas shearing.

[0008] To solve the above-mentioned technical problems, the present invention provides the following technical solution: including,

[0009] The inert gas and the sodium alginate staining solution were separately introduced into the preparation apparatus;

[0010] The sprayed solution cross-links in the receiving solution of the device to form the target microspheres.

[0011] In a preferred embodiment of the method for preparing multifaceted anisotropic microspheres based on electric assisted gas shearing according to the present invention, the inert gas includes nitrogen.

[0012] As a preferred embodiment of the method for preparing multifaceted anisotropic microspheres based on electric assisted gas shearing according to the present invention, wherein: the sodium alginate staining solution is a mixed solution of sodium alginate and macromolecular colorant, wherein the mass fraction of sodium alginate is 1-2%.

[0013] In a preferred embodiment of the method for preparing multifaceted anisotropic microspheres based on electric assisted gas shearing according to the present invention, the receiving solution is a 2% calcium chloride solution.

[0014] As a preferred embodiment of the method for preparing multifaceted anisotropic microspheres based on electric assisted gas shearing according to the present invention, the microspheres obtained by the method are homogeneous spheres with 2 to 10 faces and a particle size range of 20 to 500 μm.

[0015] The beneficial effects of this preparation method are:

[0016] This preparation method is based on the electric-assisted gas shearing method, which is simple, green, and efficient. All materials used are bio-based and biodegradable, and the resulting microspheres have small and uniform particle size. Based on these advantages, the multifaceted anisotropic microspheres prepared by this method have a wider range of potential applications.

[0017] Another objective of this invention is to overcome the shortcomings of the prior art and provide an apparatus for preparing multifaceted anisotropic microspheres based on electrically assisted gas shearing.

[0018] To solve the above-mentioned technical problems, the present invention provides the following technical solution: including,

[0019] The preparation unit includes a gas channel and a solution channel, wherein the gas channel outlet and the solution channel outlet can be arranged in four different configurations.

[0020] The receiving unit includes a copper coil and a solution receiving platform. The solution receiving platform is located directly below the gas channel outlet, and the copper coil is located between the gas channel outlet and the solution receiving platform.

[0021] As a preferred embodiment of the device for preparing multifaceted anisotropic microspheres based on electric assisted gas shearing according to the present invention, wherein: the gas channel is made of copper and has a length of 1.0 to 2.0 cm; the solution channel is composed of multiple needles, which pass through and are bound by rubber capillaries.

[0022] As a preferred embodiment of the apparatus for preparing multifaceted anisotropic microspheres based on electrically assisted gas shearing according to the present invention, the four arrangement forms of the gas channel outlet and solution channel outlet include:

[0023] The gas channel outlet is flush with the solution channel outlet;

[0024] The solution channel outlet is 0.2–1.0 mm lower than the gas channel outlet;

[0025] The solution channel outlet is 0.2–1.0 mm higher than the gas channel outlet;

[0026] The gas channel ends inward by 0.1–0.5 mm.

[0027] The beneficial effects of this preparation apparatus:

[0028] The device is simple, safe, and highly expandable.

[0029] Another objective of this invention is to overcome the shortcomings of the prior art and provide a system for preparing multifaceted anisotropic microspheres based on electrically assisted gas shearing.

[0030] To solve the above-mentioned technical problems, the present invention provides the following technical solution: comprising a preparation apparatus, and further comprising...

[0031] The control unit, used to control the reaction conditions of the preparation device, includes a high-voltage electrostatic power supply connected to the gas channel, a flow rate regulating valve, and a micro-injector connected to the inlet of the solution channel.

[0032] The analysis unit is used to analyze the microspheres prepared by the apparatus under different reaction conditions.

[0033] As a preferred embodiment of the system for preparing multifaceted anisotropic microspheres based on electrically assisted gas shearing according to the present invention, the control unit includes:

[0034] The reaction voltage is controlled to be 5–18V by the high-voltage electrostatic power supply.

[0035] The inert gas flow rate is controlled to be 1.0–8.0 L / min by the flow rate regulating valve;

[0036] The solution injection rate is controlled to be 1.0–2.0 mL / h using the microsyringe.

[0037] It also includes controlling the radius of the copper coil to be 2.0 to 4.0 cm and controlling the distance between the solution receiving platform and the gas channel outlet to be 5 to 15 cm.

[0038] The beneficial effects of this preparation system:

[0039] This invention pioneers a preparation system for multifaceted anisotropic microspheres based on electrically assisted gas shearing. The system produces target microspheres with a particle size of less than 100 μm that still retain a multifaceted anisotropic microsphere structure. The particle size of the microspheres can be controlled by adjusting the high-voltage electrostatic voltage, gas flow rate, solution injection rate, coil diameter, distance between the solution receiving platform and the gas channel outlet, and the arrangement of the gas and solution channel outlets. The experimental equipment is simple, safe, and highly scalable. All materials used are bio-based and biodegradable. Based on these advantages, the small-particle-size anisotropic microspheres prepared by this method have a wide range of applications. Attached Figure Description

[0040] To more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the following description of the embodiments will be briefly introduced. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort. Wherein:

[0041] Figure 1 J is the device for preparing multifaceted anisotropic microspheres based on electrically assisted gas shearing in this invention.

[0042] Figure 2 This is a schematic diagram of the multifaceted needle of the present invention.

[0043] Figure 3 This is a diagram showing the arrangement of the gas channel outlet and the solution channel outlet of the present invention.

[0044] Figure 4 This is a schematic diagram of the system for preparing multifaceted anisotropic microspheres based on electric-assisted gas shearing, as provided by the present invention.

[0045] Figure 5 This is a schematic diagram of the control unit in the system for preparing multifaceted anisotropic microspheres according to the present invention.

[0046] Figure 6 These are microscope images and particle size distribution diagrams of microspheres prepared at different voltages in Example 4 of the present invention. Detailed Implementation

[0047] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, the specific embodiments of the present invention will be described in detail below with reference to the examples in the specification.

[0048] Many specific details are set forth in the following description in order to provide a full understanding of the invention. However, the invention may also be practiced in other ways different from those described herein, and those skilled in the art can make similar extensions without departing from the spirit of the invention. Therefore, the invention is not limited to the specific embodiments disclosed below.

[0049] Secondly, the term "one embodiment" or "embodiment" as used herein refers to a specific feature, structure, or characteristic that may be included in at least one implementation of the present invention. The phrase "in one embodiment" appearing in different places in this specification does not necessarily refer to the same embodiment, nor is it a single or selective embodiment that is mutually exclusive with other embodiments.

[0050] Example 1

[0051] As a first embodiment of the present invention, a method for preparing multifaceted anisotropic microspheres based on electric assisted gas shearing is provided.

[0052] S1: Prepare the required solution.

[0053] A1: Preparation of sodium alginate solution: Weigh 1.5g of sodium alginate and dissolve it in 100mL of deionized water to obtain a 1.5% sodium alginate solution. Dispense the solution into 10mL portions and add 2-3 drops of macromolecular dye for staining to obtain sodium alginate staining solution.

[0054] A2: Prepare calcium chloride solution: Accurately weigh 2g of calcium chloride and dissolve it in 100ml of deionized water to obtain a 2% calcium chloride solution.

[0055] S2: Inert gas and sodium alginate staining solution are respectively pushed into device J.

[0056] Specifically, sodium alginate staining solution is injected into the device through the solution channel using a micro-syringe, and inert gas is injected into the device through the gas channel on the side of the device.

[0057] S3: The solution enters the receiving solution under the action of gas shear force and electrostatic force to cross-link into spheres.

[0058] Specifically, the microspheres are controlled by adjusting the reaction voltage, airflow speed, solution injection speed, coil diameter, distance between the solution receiving platform and the gas channel outlet, and the number of solution channel needles, thereby obtaining the target microspheres.

[0059] Example 2

[0060] Reference Figures 1-3 This is the second embodiment of the present invention, which illustrates a device J for preparing multifaceted anisotropic microspheres based on electrically assisted gas shearing. Figure 1 This device includes a preparation unit 100 and a receiving unit 200.

[0061] The preparation unit includes a gas channel 101 and a solution channel 102, with the solution channel located at the center of the gas channel to ensure that the gas shear force on the droplets is balanced.

[0062] Specifically, the gas channel is made of copper, with a channel length of 1.0–2.0 cm, and uses needles with a specification range of 14–20 G; the solution channel consists of multiple needles with a specification range of 22–34 G. Figure 2 All needles are bound together by rubber capillaries to prevent them from scattering. When the number of needles exceeds 6, the gray needle in the middle is used to help fix the solution needles around it. This needle does not pass through the solution.

[0063] Furthermore, it can be seen Figure 3 The gas channel 101 outlet and the solution channel 102 outlet can be arranged in four different configurations to adjust the microsphere size, including...

[0064] The outlet of gas channel 101 is flush with the outlet of solution channel 102;

[0065] The outlet of solution channel 102 is 0.2–1.0 mm lower than the outlet of gas channel 101;

[0066] The outlet of solution channel 102 is 0.2–1.0 mm higher than the outlet of gas channel 101;

[0067] The gas channel 101 tapers inward at its end by 0.1–0.5 mm;

[0068] The receiving unit 200 includes a copper coil 201 and a solution receiving platform 202;

[0069] Specifically, the solution receiving platform 202 is located directly below the outlet of the gas channel 101, and the copper coil 201 is located between the outlet of the gas channel 101 and the solution receiving platform 202.

[0070] Example 3

[0071] See Figures 4-5 This is the third embodiment of the present invention, which illustrates a system for preparing multifaceted anisotropic microspheres using apparatus J. Specifically, it can be seen that... Figure 4 This invention improves a system for preparing multifaceted anisotropic microspheres based on electrically assisted gas shearing. The system includes apparatus J, and also includes...

[0072] Control unit 300 is used to control the reaction conditions of the preparation apparatus, as can be seen. Figure 5 It includes a high-voltage electrostatic power supply 301 connected to the gas channel, a flow rate regulating valve 302, and a micro-injector 303 connected to the inlet of the solution channel 102.

[0073] Analysis unit 400 is used to analyze microspheres prepared by apparatus J under different reaction conditions.

[0074] Specifically, in the inert gas and sodium alginate solution injection device J, the control unit 300 regulates the microspheres by adjusting the high voltage electrostatic voltage, airflow speed, solution injection speed, coil diameter, and distance between the solution receiving platform and the gas channel outlet.

[0075] Furthermore, the microspheres obtained by adjusting different parameter conditions were observed and recorded under a microscope, and the process parameters for preparing the target microspheres were analyzed.

[0076] Example 4

[0077] See Figure 6 This is the fourth embodiment of the present invention. To verify the beneficial effects of the present invention, a practical application of a system for preparing multifaceted anisotropic microspheres using device J is provided.

[0078] Nitrogen gas and sodium alginate staining solution were separately introduced into device J. 2% calcium chloride solution was used as the receiving solution. The gas flow rate was set to 2 L / min, the solution injection rate was 1.0 mL / h, the copper coil radius was 2 cm, the distance between the solution receiving platform and the gas channel outlet was 5 cm, an octagonal needle was selected, and the reaction voltage was set to 5, 8, 10, 12, and 15 kV.

[0079] The microspheres were observed under a microscope, and their sizes were recorded to analyze the relationship between the reaction voltage and the microsphere size. Figure 6 By adjusting the voltage, microspheres with diameter distributions ranging from 20 to 350 μm can be obtained.

[0080] Analysis showed that when the high voltage electrostatic voltage was 12kV, the average diameter of the microspheres was 64.1μm, and the microspheres were uniform in size and regular in shape. When the high voltage electrostatic voltage was 15kV, the average diameter of the microspheres was 38.4μm, and the microsphere particle size decreased significantly, but the regularity of the microspheres also decreased. Therefore, a reaction voltage of 12kV was selected to prepare octahedral anisotropic microspheres with uniform particle size and regular shape.

[0081] Example 5

[0082] As a fifth embodiment of the present invention, and to verify the beneficial effects of the present invention, a practical application of a system for preparing multifaceted anisotropic microspheres using device J is provided.

[0083] Nitrogen gas and sodium alginate staining solution were separately introduced into device J. 2% calcium chloride solution was used as the receiving solution. The reaction voltage was set to 5kV, the gas flow rate to 2L / min, the radius of the copper coil to 2cm, and the distance between the solution receiving platform and the gas channel outlet to 5cm. An octagonal needle was used, and the solution introduction rates were set to 1.0mL / h, 1.2mL / h, 1.4mL / h, 1.6mL / h, 1.8mL / h, and 2.0mL / h.

[0084] Microspheres were observed under a microscope, and their sizes were recorded to analyze the relationship between reaction voltage and microsphere size. By adjusting the solution injection rate, microspheres with diameter distributions ranging from 50 to 400 μm could be obtained.

[0085] Analysis showed that when the solution injection rate was 1.0 mL / h, the microsphere diameter was 300 ± 10 μm, and the microspheres were uniform in size and regular in shape. When the solution injection rate was 2.0 mL / h, the microsphere diameter was 110 ± 5 μm, and the microsphere particle size decreased significantly while the shape remained regular. Therefore, a solution injection rate of 2.0 mL / h was selected to prepare octagonal anisotropic microspheres with uniform particle size and regular shape.

[0086] Example 6

[0087] As a sixth embodiment of the present invention, and to verify the beneficial effects of the present invention, a practical application of a system for preparing multifaceted anisotropic microspheres using device J is provided.

[0088] Nitrogen gas and sodium alginate staining solution were separately introduced into apparatus J, with 2% calcium chloride solution used as the receiving solution. The reaction voltage was set to 5 kV, and the solution introduction rate was 1.0 mL / h. A copper coil with a radius of 2 cm was used, and the distance between the solution receiving platform and the gas channel outlet was 5 cm. An octagonal needle was selected, and the gas flow rates were set to 2 L / min, 4 L / min, 6 L / min, and 8 L / min.

[0089] Microspheres were observed under a microscope, and their sizes were recorded to analyze the relationship between reaction voltage and microsphere size. By adjusting the gas flow rate, microspheres with diameter distributions ranging from 50 to 500 μm could be obtained.

[0090] Analysis showed that when the gas flow rate was 2 L / min, the microsphere diameter was 200 ± 10 μm, and the microspheres were uniform in size and regular in shape. When the gas flow rate was 6 L / min, the microsphere diameter was 65 ± 5 μm, and the microsphere particle size decreased significantly, but the regularity of the microspheres also decreased. Therefore, a gas flow rate of 6.0 mL / h was selected to prepare octahedral anisotropic microspheres with uniform particle size and regular shape.

[0091] Example 7

[0092] As the seventh embodiment of the present invention, and to verify the beneficial effects of the present invention, a practical application of a system for preparing multifaceted anisotropic microspheres using device J is provided.

[0093] Nitrogen gas and sodium alginate staining solution were separately introduced into device J. 2% calcium chloride solution was used as the receiving solution. The reaction voltage was set to 10kV, the gas flow rate was 6L / min, the solution injection rate was 2.0mL / h, the distance between the solution receiving platform and the gas channel outlet was 5cm, an octagonal needle was selected, and the radii of the copper coils were set to 2cm, 3cm, and 4cm respectively.

[0094] Microspheres were observed under a microscope, and their sizes were recorded to analyze the relationship between reaction voltage and microsphere size. By adjusting the solution injection rate, microspheres with diameter distributions ranging from 50 to 150 μm could be obtained.

[0095] Analysis showed that when the radius of the copper coil was 2 cm, the diameter of the microspheres was 50 ± 10 μm, and the microspheres were uniform in size and regular in shape. When the radius of the copper coil was 4 cm, the diameter of the microspheres was 140 ± 10 μm, and the microspheres were also uniform in size and regular in shape. Therefore, a copper coil radius of 2 cm was selected to prepare octagonal anisotropic microspheres with uniform particle size and regular shape.

[0096] Example 8

[0097] As the eighth embodiment of the present invention, and to verify the beneficial effects of the present invention, a practical application of a system for preparing multifaceted anisotropic microspheres using device J is provided.

[0098] Nitrogen gas and sodium alginate staining solution were separately introduced into device J. 2% calcium chloride solution was used as the receiving solution. The reaction voltage was set to 10kV, the gas flow rate to 6L / min, the solution injection rate to 2.0mL / h, the copper coil radius to 2cm, and an octagonal needle was selected. The distances between the solution receiving platform and the gas channel outlet were set to 5cm, 8cm, 10cm, and 15cm, respectively.

[0099] Microspheres were observed under a microscope, and their sizes were recorded to analyze the relationship between reaction voltage and microsphere size. By adjusting the solution injection rate, microspheres with diameter distributions ranging from 50 to 90 μm could be obtained.

[0100] Analysis showed that when the distance between the solution receiving platform and the gas channel outlet was 5 cm, the microsphere diameter was 50 ± 5 μm, and the microspheres were uniform in size and regular in shape. When the distance between the solution receiving platform and the gas channel outlet was 15 cm, the microsphere diameter was 80 ± 10 μm, and the microsphere particle size decreased significantly, but the regularity of the microspheres also decreased significantly. Therefore, a distance of 5 cm between the solution receiving platform and the gas channel outlet was selected to prepare octagonal anisotropic microspheres with uniform particle size and regular shape.

[0101] As can be seen, the method, apparatus, and system for preparing anisotropic microspheres based on electrically assisted gas shearing provided by this invention can prepare microspheres by combining high-voltage electrostatics and gas shearing. The target microspheres still have anisotropic microsphere structures even when the particle size is less than 100 μm. This invention can control the microsphere particle size by adjusting the high-voltage electrostatic voltage, airflow velocity, solution injection velocity, coil diameter, distance between the solution receiving platform and the gas channel outlet, and the arrangement of the gas channel and solution channel outlets. At the same time, the sodium alginate concentration is optimized. Experiments have confirmed that the microspheres prepared at the sodium alginate solution concentration of our invention have the best morphology. In addition, the experimental equipment is simple and safe, with rich scalability, and all materials used are bio-based and biodegradable. Based on these advantages, the small-particle-size anisotropic microspheres prepared by this method will have a very wide range of applications.

[0102] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit it. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all such modifications or substitutions should be covered within the scope of the claims of the present invention.

Claims

1. A method for preparing multifaceted anisotropic microspheres based on electrically assisted gas shearing, characterized in that: include, An inert gas and a sodium alginate staining solution with a mass fraction of 1-2% were separately introduced into the preparation apparatus (J); The sprayed solution cross-links in the receiving solution of the device (J) to form octagonal anisotropic microspheres with a diameter of 50±10μm, uniform particle size, and regular shape and size. The receiving solution is a 2% calcium chloride solution. The preparation apparatus (J) includes, The preparation unit (100) includes a gas channel (101) and a solution channel (102), wherein the outlet of the gas channel (101) and the outlet of the solution channel (102) can be changed into four different arrangement forms; The gas channel (101) is made of copper and has a length of 1.0~2.0cm; the solution channel (102) is composed of multiple needles, which pass through a rubber capillary tube and are bound thereto. The receiving unit (200) includes a copper coil (201) and a solution receiving platform (202). The solution receiving platform (202) is located directly below the outlet of the gas channel (101), and the copper coil (201) is located between the outlet of the gas channel (101) and the solution receiving platform (202). The control unit (300) is used to control the reaction conditions of the preparation device (J), including a high voltage electrostatic power supply (301) connected to the gas channel (101), a flow rate regulating valve (302), and a micro-injector (303) connected to the inlet of the solution channel (102). The reaction voltage of the device (J) is set to 10 kV, the gas flow rate is 6 L / min, the solution injection rate is 2.0 mL / h, the distance between the solution receiving platform and the gas channel outlet is 5 cm, an octagonal needle is selected, and the radius of the copper coil is set to 2 cm.

2. The method for preparing multifaceted anisotropic microspheres based on electrically assisted gas shearing as described in claim 1, characterized in that: The inert gas is nitrogen.

3. The method for preparing multifaceted anisotropic microspheres based on electrically assisted gas shearing as described in claim 1, characterized in that: The sodium alginate staining solution is a mixed solution of sodium alginate and macromolecular colorant.

4. The method for preparing multifaceted anisotropic microspheres based on electrically assisted gas shearing as described in claim 1, characterized in that: The four arrangement forms of the gas channel (101) outlet and the solution channel (102) outlet include, The outlet of the gas channel (101) is flush with the outlet of the solution channel (102); The outlet of the solution channel (102) is 0.2~1.0 mm lower than the outlet of the gas channel (101); The outlet of the solution channel (102) is 0.2~1.0 mm higher than the outlet of the gas channel (101); The gas channel (101) is narrowed inward by 0.1~0.5mm at the end.

5. The method for preparing multifaceted anisotropic microspheres based on electrically assisted gas shearing as described in claim 1, characterized in that: The device (J) further includes, The analysis unit (400) is used to analyze the microspheres prepared by the apparatus (J) under different reaction conditions.

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