Ultrasonic-assisted micro-reaction device for preparing nanoparticles
By introducing an ultrasonic-assisted microreactor for nanoparticle preparation into the solution condensation method, combined with a capillary spiral flow channel and a constant temperature water bath system, the problem of the inability of existing devices to accurately control the size of nanoparticles was solved, and uniform nucleation and efficient preparation of nanoparticles were achieved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-28
- Publication Date
- 2026-03-06
AI Technical Summary
Existing solutions-based polymer nanoparticle production equipment lacks temperature control systems and pH monitoring devices, making it impossible to precisely control the size of nanoparticles.
A microreactor for preparing nanoparticles with ultrasound assistance was designed. It uses a capillary spiral flow channel and an ultrasonic transducer, combined with a constant temperature water bath and sensors, to achieve real-time monitoring and control of reaction temperature and pH value. Ultrasound promotes the nucleation of nanoparticles and controls the particle size.
Uniform nucleation and efficient preparation of nanoparticles were achieved, ensuring the uniformity of nanoparticle size and the stability of the reaction, making it suitable for industrial production.
Smart Images
Figure CN223969957U_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of solution-based nanoparticle preparation technology, and in particular to a microreactor for ultrasonic-assisted nanoparticle preparation. Background Technology
[0002] Particles with a size ranging from 1 to 100 nm are called nanoparticles. Nanoparticles possess a large specific surface area and exhibit novel properties and functions not found in materials with sizes larger than micrometers. Currently, nanopolymer materials have been applied in many fields, such as controlled drug release carriers, immunoassay, and interventional diagnostics, due to their unique and excellent properties. The size of nanoparticles has a significant impact on their properties. By adjusting the size and shape of nanoparticles, their optical, magnetic, and catalytic properties can be precisely controlled, providing an important foundation for the application of nanotechnology.
[0003] In immunoassays, the selection of carrier materials is crucial. Polymer nanoparticles, especially those with hydrophilic surfaces, exhibit minimal adsorption of non-specific proteins and are therefore widely used as novel labeling carriers. In controlled drug release, nanoparticles made from polymers such as polylactic acid, lactic acid-glycolic acid copolymers, and polyacrylates have significant application value. They can protect drugs and control their release rate, minimizing drug efficacy loss after transport and effectively controlling release, thus prolonging the duration of action. Drug carriers made from nanopolymers can load or encapsulate various drugs, whether hydrophilic, hydrophobic, or biomolecules, while effectively controlling the release rate. Nanoparticles can be obtained through various methods, including microemulsion polymerization, solution precipitation, and solution coagulation. The microemulsion method requires the addition of a large amount of surfactants and non-aqueous solvents or dispersants during the preparation process. The solution precipitation method is mainly used for the preparation of inorganic nanoparticles, while the solution coagulation method does not require the addition of surfactants and can prepare a large number of polymer nanoparticles, which is easy to industrialize. However, it has the disadvantage of difficult particle size control and large deviation, which limits its use.
[0004] Solution coagulation can control the size of polymer nanoparticles through reaction conditions. Temperature is a crucial factor affecting polymer particle size; increased temperature leads to faster molecular chain movement and reaction rate, thus influencing particle size. pH changes also affect particle size. Generally, higher pH values result in smaller average particle sizes, while lower pH values lead to larger average particle sizes. The presence of electrolytes also affects particle size. However, existing polymer nanoparticle preparation devices lack temperature control systems and pH monitoring devices, making precise control of the produced polymer particle size impossible. Utility Model Content
[0005] To address the problem that existing solution-coagulation methods for producing polymer nanoparticles lack temperature control and pH monitoring devices, thus hindering precise control of the produced polymer particle size, this invention provides an ultrasonic-assisted microreactor for preparing nanoparticles, thereby resolving the issues raised in the background section.
[0006] The technical solution of this utility model is:
[0007] A microreactor for ultrasonic-assisted preparation of nanoparticles includes a reaction liquid storage tank I, a reaction liquid storage tank II, a peristaltic pump I, a peristaltic pump II, a Y-connector, a water bath, a capillary spiral flow pipe, an ultrasonic transducer, and a nanoparticle solution storage tank.
[0008] The outlets of reaction liquid storage tank I and reaction liquid storage tank II are connected to the inlet of Y-type connector through peristaltic pump I and peristaltic pump II, respectively. The outlet of Y-type connector is connected to the inlet of capillary spiral flow pipe. The capillary spiral flow pipe is installed in water bath tank. Multiple ultrasonic transducers are installed on the side wall and bottom of water bath tank. The outlet of capillary spiral flow pipe is connected to nanoparticle solution storage tank.
[0009] Furthermore, the inner diameter of the capillary spiral flow channel is 0.5-1.5 mm.
[0010] Furthermore, the ultrasonic transducers located on the side wall of the water bath are arranged on the same plane.
[0011] Furthermore, the ultrasonic transducer located on the side wall of the water bath is positioned below the coolant level.
[0012] Furthermore, it also includes a constant temperature water bath device, the outlet of which is connected to the water bath tank via a water bath device flow pump.
[0013] Furthermore, the constant temperature water bath device is equipped with a temperature regulation device.
[0014] Furthermore, the temperature regulating device is a semiconductor refrigeration chip.
[0015] Furthermore, a pH sensor is provided at the outlet of the capillary spiral flow channel.
[0016] Furthermore, a temperature sensor is installed inside the water bath tank.
[0017] Furthermore, the outlet of the capillary spiral flow pipe is also connected to a waste liquid storage tank.
[0018] Compared with the prior art, the present invention has the following advantages:
[0019] 1. A microreactor for ultrasonic-assisted preparation of nanoparticles, employing a capillary spiral flow channel as the reaction site for the mixed liquid, enabling continuous and controllable mass preparation of nanoparticles. An ultrasonic transducer is installed to emit ultrasonic waves into the capillary spiral flow channel. The ultrasonic waves promote the nucleation of nanoparticles, generating a large number of nanoparticle cores in a short time. Compared to reactions in straight tubes, the capillary spiral flow channel increases the contact time between the reaction solution and the ultrasonic waves at the same flow rate, ensuring thorough mixing of the reaction liquid. The ultrasonic waves generated by the transducer induce cavitation in the liquid inside the capillary spiral flow channel of the microreactor, enhancing liquid mixing and reaction while preventing clogging.
[0020] 2. A water bath is provided to cool the capillary spiral flow channel. A constant-temperature water bath device with a semiconductor cooling chip maintains a constant water temperature. Because ultrasound can cause the reactant solution temperature to rise, leading to larger nanoparticles and uneven product nanoparticle diameters, a water bath is used to cool the capillary spiral flow channel to ensure a constant reaction solution temperature. Compared to reactions in a straight tube, the capillary spiral flow channel increases the contact area with the water bath, further improving cooling efficiency.
[0021] 3. A control device is provided to adjust the diameter of nanoparticles by controlling the power of the ultrasonic transducer. The control device monitors the pH sensor and temperature sensor to further adjust the reactant ratio and the temperature of the constant temperature water bath to ensure the normal progress of the reaction. Attached Figure Description
[0022] Figure 1 This is a schematic diagram of the structure of this utility model;
[0023] Figure 2 Schematic diagram of the water bath tank Figure I ;
[0024] Figure 3 Schematic diagram of the water bath tank Figure II ;
[0025] Figure 4 This is a schematic diagram of the structure of a water bath tank and a capillary spiral flow pipe.
[0026] In the diagram: 101, Reaction liquid storage tank I; 102, Reaction liquid storage tank II; 103, Peristaltic pump I; 104, Peristaltic pump II; 105, Y-type connector; 201, Water bath tank; 202, Capillary spiral flow pipe; 203, Ultrasonic transducer; 204, Nanoparticle solution storage tank; 301, Constant temperature water bath device; 302, Temperature regulating device; 303, Water bath device flow pump; 4, pH sensor; 5, Temperature sensor; 6, Waste liquid storage tank; 7, Control device. Detailed Implementation
[0027] Specific implementation method one: See Figure 1-4 As shown, a microreactor for ultrasonic-assisted preparation of nanoparticles includes a reaction liquid storage tank I 101, a reaction liquid storage tank II 102, a peristaltic pump I 103, a peristaltic pump II 104, a Y-type connector 105, a water bath 201, a capillary spiral flow pipe 202, an ultrasonic transducer 203, and a nanoparticle solution storage tank 204.
[0028] The outlets of reaction liquid storage tanks I101 and II102 are connected to the inlet of Y-type connector 105 via peristaltic pump I103 and peristaltic pump II104, respectively. The outlet of Y-type connector 105 is connected to the inlet of capillary spiral flow pipe 202. The capillary spiral flow pipe 202 is installed in water bath tank 201. Multiple ultrasonic transducers 203 are installed on the side wall and bottom of water bath tank 201. The outlet of capillary spiral flow pipe 202 is connected to nanoparticle solution storage tank 204.
[0029] Furthermore, the Y-connector 105 serves to mix the reactants. The water bath 201 contains cooling water, and the capillary spiral flow pipe 202 is installed below the liquid surface. An ultrasonic transducer 203 is fixed to the outer wall of the water bath 201, with its sound-emitting surface facing inwards. One ultrasonic transducer 203 is installed on each of the left and right side walls of the water bath 201, and two ultrasonic transducers 203 are installed on the bottom and front and rear side walls of the water bath 201. The power of the ultrasonic transducers 203 is set to 800W. The reaction solution flows through the Y-connector 105 for mixing and is then pumped into the capillary spiral flow pipe 202, where it is mixed and reacted through ultrasonic vibration. Ultrasound can promote the nucleation of nanoparticles, generating a large number of nanoparticle cores in a short time. Compared with the reaction in a straight tube, the capillary spiral flow channel 202 increases the contact time between the reaction solution and the ultrasound at the same flow rate, allowing the reaction liquid to be fully mixed. The ultrasound generated by the ultrasonic transducer 202 will cause the liquid inside the capillary spiral flow channel of the microreactor to produce a cavitation effect, which will enhance the mixing and reaction of the liquid and prevent clogging.
[0030] Specific Implementation Method Two: See Figure 4 As shown, the inner diameter of the capillary spiral flow channel 202 in this embodiment is 0.5-1.5 mm.
[0031] Specific implementation method three: See Figure 4 As shown, in this embodiment, the ultrasonic transducer 203 located on the side wall of the water bath tank 201 is arranged on the same plane.
[0032] Furthermore, the inner diameter of the capillary spiral flow channel 202 is preferably 1 mm, and the outer diameter is 2 mm. Since ultrasound transmits energy through cooling water, the ultrasonic transducer 203 is positioned below the liquid surface of the water bath 201. The ultrasonic transducers 203 are positioned on the same plane, ensuring that the distance between the ultrasonic transducers 203 located on the side wall of the water bath 201 and the capillary spiral flow channel 202 is equal. This ultrasonic vibration of the reaction liquid leads to more uniform nanoparticle products. Because ultrasound can cause the temperature of the reactant solution to rise, resulting in larger nanoparticles and uneven nanoparticle diameters, a water bath is used to cool the capillary spiral flow channel to ensure a constant reaction solution temperature. Compared to reactions in a straight pipe, the capillary spiral flow channel increases the contact area with the water bath, further improving cooling efficiency.
[0033] Detailed Implementation Method Four: See [link] Figure 1 As shown, in this embodiment, the ultrasonic transducer (203) located on the side wall of the water bath tank (201) is positioned below the surface of the coolant. The reaction liquid storage tank I 101 contains N-2-HACC solution, and the reaction liquid storage tank II 102 contains CMCS solution. The peristaltic pump I 103 and the peristaltic pump II 104 control the mixing ratio of N-2-HACC and CMCS to be 1:1-1:5.
[0034] Specific implementation method five: See Figure 1 As shown, this embodiment also includes a constant temperature water bath device 301, which is equipped with a temperature regulating device 302. The outlet of the constant temperature water bath device 301 is connected to the water bath tank 201 through a water bath device flow pump 303.
[0035] Specific implementation method six: See Figure 1 As shown, the temperature regulating device 302 in this embodiment is a semiconductor refrigeration chip.
[0036] Detailed implementation method seven: See Figure 1 As shown, the temperature of the water output from the water bath device 301 in this embodiment is 20-25°C.
[0037] Furthermore, the constant temperature water bath device 301 uses a closed-loop circulation pipe to cool the cooling water, so a single water bath device flow pump 303 can achieve the outflow and return of the cooling water. The closed-loop circulation pipe in the constant temperature water bath device 301 is cooled by a semiconductor cooling chip.
[0038] Detailed Implementation Method Eight: See also Figure 1 As shown, a pH sensor 4 is provided at the outlet of the capillary spiral flow pipe 202 in this embodiment.
[0039] Detailed Implementation Method Nine: See also Figure 1As shown, a temperature sensor 5 is installed inside the water bath tank 201 in this embodiment.
[0040] Furthermore, a control device is provided to adjust the diameter of the nanoparticles by controlling the power of the ultrasonic transducer. The control device also monitors the pH and temperature sensors to adjust the reactant ratio and the temperature of the constant temperature water bath to ensure the normal progress of the reaction.
[0041] Detailed Implementation Method Ten: See [link] Figure 1 As shown, the outlet of the capillary spiral flow pipe 202 in this embodiment is also connected to a waste liquid storage tank 6, which is used to collect deionized water used for cleaning the pipe.
[0042] During operation, the ultrasonic transducer 203 and the constant temperature water bath device 301 are activated, with the output water temperature controlled at 25℃. Peristaltic pumps I 103 and II 104 are activated to pump N-2-HACC and CMCS solutions from reaction solution storage tanks I 101 and II 102, respectively. The reaction solutions flow through Y-connector 105 for mixing and are then pumped into capillary spiral flow pipeline 202 for further mixing and reaction. After the reaction is complete, the reaction products are collected through nanoparticle solution storage tank 204. After operation, all reaction pipelines are cleaned with deionized water, and deionized water is collected in waste liquid storage tank 12.
[0043] The above embodiments are only used to illustrate the technical solutions of this utility model, and are not intended to limit it. Although this utility model 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. Such 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 this utility model.
Claims
1. An ultrasonic-assisted microreactor for the preparation of nanoparticles, characterized in that it comprises: The capillary spiral flow pipe (202) is installed in the water bath tank (201), a plurality of ultrasonic transducers (203) are installed on the side wall and the bottom of the water bath tank (201), and the outlet of the capillary spiral flow pipe (202) is communicated with the nanoparticle solution storage tank (204). The water outlets of the reaction liquid storage tank I (101) and the reaction liquid storage tank II (102) are respectively communicated with the water inlets of the peristaltic pump I (103) and the peristaltic pump II (104) and the water outlet of the Y-shaped joint (105), the water outlet of the Y-shaped joint (105) is communicated with the inlet of the capillary spiral flow pipe (202), the capillary spiral flow pipe (202) is installed in the water bath tank (201), a plurality of ultrasonic transducers (203) are installed on the side wall and the bottom of the water bath tank (201), and the outlet of the capillary spiral flow pipe (202) is communicated with the nanoparticle solution storage tank (204).
2. The microreactor for the ultrasound-assisted nanoparticle preparation according to claim 1, characterized in that: The inner diameter of the capillary spiral flow pipe (202) is 0.5-1.5mm.
3. The microreactor for the ultrasound-assisted nanoparticle preparation according to claim 1, characterized in that: The ultrasonic transducers (203) located on the side wall of the water bath tank (201) are arranged on the same plane.
4. The microreactor for the ultrasound-assisted nanoparticle preparation according to claim 1, characterized in that: The ultrasonic transducers (203) located on the side wall of the water bath tank (201) are arranged below the liquid level of the cooling liquid.
5. The microreactor for the ultrasound-assisted nanoparticle preparation according to claim 1, wherein: The water outlet of the constant temperature water bath device (301) is communicated with the water bath tank (201) through the water bath device flow pump (303).
6. The microreactor for the ultrasound-assisted nanoparticle preparation according to claim 5, characterized in that: The constant temperature water bath device (301) is provided with a temperature adjusting device (302).
7. The microreactor for the ultrasound-assisted nanoparticle production according to claim 6, characterized in that: The temperature adjusting device (302) is a semiconductor refrigeration sheet.
8. The microreactor for the ultrasound-assisted nanoparticle production according to claim 1, characterized in that: The outlet of the capillary spiral flow pipe (202) is provided with a pH sensor (4).
9. The microreactor for the ultrasound-assisted nanoparticle production according to claim 1, characterized in that: The water bath tank (201) is provided with a temperature sensor (5).
10. The microreactor for the ultrasound-assisted nanoparticle production according to claim 1, characterized in that: The outlet of the capillary spiral flow pipe (202) is also communicated with a waste liquid storage tank (6). The water bath tank (201) is provided with a temperature sensor (5).