Liquid sample injection and synchronous mixing method based on magnetic force driving reinforcement

Abstract

The application belongs to the field of new chemical equipment, and discloses a liquid sampling and synchronous mixing method based on magnetic driving reinforcement. The liquid distributor is driven to move by a rotating magnetic field, and the liquid to be added is dispersed into the main phase through the internal flow channel of the liquid distributor, and the liquid distributor rotates while stirring the liquid to realize efficient mixing and dispersion. The liquid distributor is a curved polygon, including a dispersion part and a magnetic control part, a liquid tank and a flow channel of the dispersion part, and the magnetic control part is located at the bottom of the dispersion part. The magnetic driving mixing sampling method can realize continuous and uniform dispersion of the liquid to be added on the surface of the main phase, and efficient mixing under the stirring of the magnetic control part of the liquid distributor. Compared with the direct drop method, the sampling speed of the application is controllable, the sampling point dispersion is located at the high-speed rotating point of the liquid distributor, the liquid dispersion and efficient mixing are realized synchronously, the local concentration near the sampling point is directly and efficiently consumed, and the key problem of too high local concentration caused by direct drop is avoided.

Description

Technical Field

[0001] This invention belongs to the field of new chemical equipment and relates to liquid sampling methods, specifically a liquid sampling and synchronous mixing method based on magnetic drive enhancement. Background Technology

[0002] In liquid-phase reactions or crystallization, the addition of liquid is a crucial step. Traditional dropwise addition methods result in local concentrations near the addition point that are significantly higher than the bulk concentration. In liquid-phase reactions, this leads to excessively high reaction rates near the addition point, increasing the likelihood of side reactions. In exothermic reactions, it can cause excessively high local temperatures. In liquid-phase crystallization, excessively high local concentrations result in extremely high supersaturation, making explosive nucleation highly likely and leading to dispersed crystal particles and poor morphology. Furthermore, in published literature and patents regarding stirring and addition devices, addition is often done directly dropwise, and stirring and addition are usually performed independently. This method results in the addition point being out of sync with the high-speed rotation of the stirrer, leading to low stirring efficiency.

[0003] Therefore, it is necessary to develop a new method of sample addition and liquid-phase mixing to reduce the local concentration near the sample addition point, so as to avoid the adverse effects of the traditional sample addition method on the liquid-phase reaction or crystallization process. Summary of the Invention

[0004] To address the issues of excessively high local concentrations near the sample addition point and low stirring efficiency resulting from independent sample addition and stirring in direct dropwise addition methods, this invention proposes a magnetically driven, enhanced liquid addition and simultaneous mixing method. This method uses a rotating magnetic field to drive a liquid distributor to rotate within the bulk phase. The liquid to be added to the distributor's tank is dispersed and discharged into the bulk phase through multiple channels connected to the tank under the influence of centrifugal force, gravity, and surface tension. Simultaneously, the rotating liquid distributor stirs the liquid, promoting mixing between the two phases. Furthermore, by adjusting the frequency of the rotating magnetic field, the rotation speed of the liquid distributor can be controlled, further regulating the dispersion rate of the added liquid and the mixing intensity within the bulk phase.

[0005] The technical solution of the present invention:

[0006] A method for simultaneous mixing of liquids by magnetically driven addition includes the following steps:

[0007] (1) Design of liquid distributor:

[0008] The main structure of the liquid distributor is a curved polygon with a certain thickness; this curved polygon is a rotationally symmetric structure containing 2-8 corners; the liquid distributor is divided into a dispersion section and a magnetic control section. The dispersion section includes a liquid tank and flow channels; the flow channels are inclined flow channels, with the inclination direction being the direction in which the height of the dispersion section decreases, and the inclination angle being 1°-30°, and the flow channels are distributed on one or more corners; the liquid tank is circular and located at the center of the dispersion section, and the bottom of the liquid tank is connected to all flow channels; the magnetic control section is located in a sealed groove at the center of the bottom of the dispersion section, and the sealed groove is filled with magnetic material;

[0009] (2) Manufacturing of liquid distributor:

[0010] By 3D printing the dispersion part and the magnetron part, magnetic material is added into the groove, and then the dispersion part and the magnetron part are combined into one piece by ultraviolet light curing.

[0011] The magnetic material is one or a mixture of two or more of the following: iron oxide powder, neodymium iron boron powder, and chromium dioxide powder.

[0012] (3) Perform liquid dispersion:

[0013] 1) Add the bulk liquid phase to the reaction vessel;

[0014] 2) Place the liquid distributor in the reaction vessel, with the magnetron submerged in the bulk liquid phase and the dispersion section exposed above the surface of the bulk liquid phase;

[0015] 3) Transfer the reaction vessel to the platform of the three-dimensional magnetic field generator;

[0016] 4) After adding the liquid to be dispersed into the micropipette, suspend the micropipette above the liquid tank corresponding to the liquid distributor;

[0017] 5) Turn on the rotating magnetic field and set the magnetic field strength and frequency;

[0018] 6) After the liquid distributor has been rotating stably for a period of time and a stable flow field has been formed in the bulk liquid phase, the liquid to be dispersed is dripped into the liquid tank of the liquid distributor through a micro-syringe.

[0019] 7) The added dispersed liquid is dispersed and discharged through the inclined flow channel connected to the liquid distributor under the combined action of gravity, centrifugal force and surface tension, and enters the main liquid phase. At the same time, the magnetic control unit stirs to promote the mixing of the two phases.

[0020] The beneficial effects of this invention are as follows: By driving the liquid distributor to rotate using a magnetic field, the droplets in the liquid tank are dispersed into multiple streams through multiple curved flow channels, continuously entering the bulk phase at the point of maximum rotational linear velocity, greatly reducing the local high concentration caused by direct drop addition; the sample addition point is the same as the rapid rotation point of the liquid distributor, directly and efficiently consuming the local concentration near the dispersion point, avoiding the adverse effects of direct drop addition on the liquid phase reaction or crystallization process. Simultaneously, the use of an external magnetic field control allows for higher device rotation speed and greater adjustability, which can enhance the mixing of the liquid to be dispersed with the bulk phase. Attached Figure Description

[0021] Figure 1 This is a schematic diagram of the method.

[0022] Figure 2 A schematic diagram of the curved pentagonal liquid distributor designed for this method is shown in (a) front view, (b) side view, and (c) top view.

[0023] Figure 3 A schematic diagram of the curved triangular liquid distributor designed for this method is shown in (a) front view, (b) side view, and (c) top view.

[0024] Figure 4 A physical diagram of a liquid distributor designed for this method.

[0025] In the figure: 1 Micro-pipette, 2 Liquid distributor, 3 Magnetic field generator, 4 Groove of the magnetic control section, 5 Flow channel of the dispersion section, 6 Magnetic control section as a whole, 7 Dispersion section as a whole, 8 Liquid tank of the dispersion section. Detailed Implementation

[0026] The specific embodiments of the present invention will be further described below with reference to the accompanying drawings and technical solutions.

[0027] Example 1

[0028] Manufacturing the liquid distributor: A 3D model of the liquid distributor is created in 3D modeling software. The liquid distributor in this embodiment is shown in the attached figure. Figure 2 As shown, the design is a curved pentagon with a circumscribed circle diameter of 16mm. The overall height of the dispersion section 7 is 2mm, and each of the five corners has an inclined flow channel 5. The liquid tank 8 has a diameter of 2mm and its bottom is connected to the five inclined flow channels at an inclination angle of 5°. The overall height of the magnetocontrol section 6 is 5mm, and a cylindrical groove 4 with a diameter of 5mm is set in the center of the pentagon. The designed dispersion section and magnetocontrol section are printed using 3D printing technology. After adding iron oxide powder into the cylindrical groove of the magnetocontrol section, the dispersion section and magnetocontrol section are bonded together by ultraviolet light curing. The actual liquid distributor is shown in the attached figure. Figure 3 As shown.

[0029] Liquid dispersion: (1) Add 5g of glycerol to a petri dish; (2) Place the liquid distributor in the petri dish, with the magnetron submerged in the glycerol and the dispersion part still exposed above the glycerol surface; (3) Transfer the petri dish to the stage of the three-dimensional magnetic field generator; (4) Add deionized water to the micro-pipette and suspend it above the liquid tank of the liquid distributor; (5) Turn on the rotating magnetic field, set the magnetic field strength to 150Gs and the magnetic field frequency to 2Hz; (6) After the liquid distributor rotates stably for 1min to form a stable flow field in the glycerol, add 20μL of water to the liquid tank of the liquid distributor through the micro-pipette; (7) Under the combined action of gravity, centrifugal force and surface tension, the added water is dispersed and discharged through the five inclined channels connected to the liquid distributor and enters the glycerol. The magnetron stirs at the same time to promote the mixing of water and glycerol.

[0030] The process of water dispersion and mixing with glycerol was recorded in real time using a camera. The results showed that the time for complete dispersion of 20 μL of water was 247 s, and the time for complete mixing of water and glycerol was 260 s.

[0031] Example 2

[0032] Manufacturing the liquid distributor: A 3D model of the liquid distributor is created in 3D modeling software. The liquid distributor in this embodiment is shown in the attached figure. Figure 2 As shown, the design is a curved pentagon with a circumscribed circle diameter of 16mm. The dispersion section 7 has an overall height of 2mm, and each of the five corners has an inclined flow channel 5. The liquid tank 8 has a diameter of 2mm and its bottom is connected to the five inclined flow channels at an inclination angle of 5°. The magnetocontrol section 6 has an overall height of 5mm, and a cylindrical groove 4 with a diameter of 5mm is set in the center of the pentagon. The designed dispersion section and magnetocontrol section are printed using 3D printing technology. After adding iron oxide powder into the cylindrical groove of the magnetocontrol section, the dispersion section and magnetocontrol section are bonded together by ultraviolet light curing.

[0033] Liquid dispersion: (1) Add 5g of glycerol to a petri dish; (2) Place the liquid distributor in the petri dish, with the magnetron submerged in the glycerol and the dispersion part still exposed above the glycerol surface; (3) Transfer the petri dish to the stage of the three-dimensional magnetic field generator; (4) Add deionized water to the micro-pipette and suspend it above the liquid tank of the liquid distributor; (5) Turn on the rotating magnetic field, set the magnetic field strength to 150Gs and the magnetic field frequency to 6Hz; (6) After the liquid distributor rotates stably for 1min to form a stable flow field in the glycerol, add 20μL of water to the liquid tank of the liquid distributor through the micro-pipette; (7) Under the combined action of gravity, centrifugal force and surface tension, the added water is dispersed and discharged through the five inclined channels connected to the liquid distributor and enters the glycerol. The magnetron stirs at the same time to promote the mixing of water and glycerol.

[0034] The process of water dispersion and mixing with glycerol was recorded in real time using a camera. The results showed that the time for complete dispersion of 20 μL of water was 10.3 s, and the time for complete mixing of water and glycerol was 170 s.

[0035] Example 3

[0036] Manufacturing the liquid distributor: A 3D model of the liquid distributor is created in 3D modeling software. The liquid distributor in this embodiment is shown in the attached figure. Figure 2 As shown, the design is a curved pentagon with a circumscribed circle diameter of 16mm. The overall height of the dispersion section 7 is 2mm, and each of the five corners has an inclined flow channel 5. The liquid tank 8 has a diameter of 2mm and its bottom is connected to the five inclined flow channels at an inclination angle of 5°. The overall height of the magnetocontrol section 6 is 5mm, and a cylindrical groove 4 with a diameter of 5mm is set in the center of the pentagon. The designed dispersion section and magnetocontrol section are printed using 3D printing technology. Neodymium iron boron powder is added to the cylindrical groove of the magnetocontrol section, and then the dispersion section and magnetocontrol section are bonded together by ultraviolet light curing.

[0037] Liquid dispersion: (1) Add 5g of glycerol to a petri dish; (2) Place the liquid distributor in the petri dish, with the magnetron submerged in the glycerol and the dispersion part still exposed above the glycerol surface; (3) Transfer the petri dish to the stage of the three-dimensional magnetic field generator; (4) Add deionized water to the micro-pipette and suspend it above the liquid tank of the liquid distributor; (5) Turn on the rotating magnetic field, set the magnetic field strength to 150Gs and the magnetic field frequency to 8Hz; (6) After the liquid distributor rotates stably for 1min to form a stable flow field in the glycerol, add 20μL of water to the liquid tank of the liquid distributor through the micro-pipette; (7) Under the combined action of gravity, centrifugal force and surface tension, the added water is dispersed and discharged through the five inclined channels connected to the liquid distributor and enters the glycerol. The magnetron stirs at the same time to promote the mixing of water and glycerol.

[0038] The process of water dispersion and mixing with glycerol was recorded in real time using a camera. The results showed that the time for complete dispersion of 20 μL of water was 5.0 s, and the time for complete mixing of water and glycerol was 100 s.

[0039] Example 4

[0040] Manufacturing the liquid distributor: A 3D model of the liquid distributor is created in 3D modeling software. The liquid distributor in this embodiment is shown in the attached figure. Figure 2As shown, the design is a curved pentagon with a circumscribed circle diameter of 16mm. The overall height of the dispersion section 7 is 2mm, and each of the five corners has an inclined flow channel 5. The liquid tank 8 has a diameter of 2mm and its bottom is connected to the five inclined flow channels at an inclination angle of 5°. The overall height of the magnetocontrol section 6 is 5mm, and a cylindrical groove 4 with a diameter of 5mm is set in the center of the pentagon. The designed dispersion section and magnetocontrol section are printed using 3D printing technology. Neodymium iron boron powder is added to the cylindrical groove of the magnetocontrol section, and then the dispersion section and magnetocontrol section are bonded together by ultraviolet light curing.

[0041] Liquid dispersion: (1) Add 5g of glycerol to a petri dish; (2) Place the liquid distributor in the petri dish, with the magnetron submerged in the glycerol and the dispersion part still exposed above the glycerol surface; (3) Transfer the petri dish to a stage fixed to the surface of a rotating permanent magnet; (4) Add deionized water to a micro-pipette and suspend it above the liquid tank of the liquid distributor; (5) Set the rotation speed of the permanent magnet to 600 rpm; (6) After the liquid distributor has been rotating stably for 1 minute to form a stable flow field in the glycerol, add 20μL of water to the liquid tank of the liquid distributor through the micro-pipette; (7) The water is dispersed and discharged through the five inclined channels connected to the liquid distributor under the combined action of gravity, centrifugal force and surface tension, and enters the glycerol. The magnetron stirs at the same time to promote the mixing of water and glycerol.

[0042] The process of water dispersion and mixing with glycerol was recorded in real time using a camera. The results showed that the time for complete dispersion of 20 μL of water was 4.1 s, and the time for complete mixing of water and glycerol was 40 s.

[0043] Example 5

[0044] Manufacturing the liquid distributor: A 3D model of the liquid distributor is created in 3D modeling software. The liquid distributor in this embodiment is shown in the attached figure. Figure 2 As shown, the design is a curved triangle with a circumcircle diameter of 16mm. The overall height of the dispersion section 7 is 2mm, and each of the five corners has an inclined flow channel 5. The liquid tank 8 has a diameter of 4mm and its bottom is connected to the five inclined flow channels at an inclination angle of 15°. The overall height of the magnetocontrol section 6 is 2.5mm, and a cylindrical groove 4 with a diameter of 6mm is set in the center of the pentagon. The designed dispersion section and magnetocontrol section are printed using 3D printing technology. Neodymium iron boron powder is added to the cylindrical groove of the magnetocontrol section, and then the dispersion section and magnetocontrol section are bonded together by ultraviolet light curing.

[0045] Liquid-phase crystallization: (1) Prepare a 0.1M sodium acetate buffer solution with pH=5.0. Use this buffer solution to prepare a 2% NaCl solution with pH=5.0, labeled as solution A; use this buffer solution to prepare a saturated sodium chloride solution with pH=1.0, labeled as solution B; use this buffer solution to prepare a lysozyme solution with a concentration of 40mg / mL and pH=5.0, labeled as solution C; (2) At 25℃, add 1mL of solution A and 1mL of solution C to a petri dish; (3) Place the liquid distributor in the petri dish, with the magnetron submerged in the mixed solution and the dispersion section still exposed above the surface of the mixed solution; (4) Place the petri dish... (3) Transfer the dish to the stage fixed on the surface of the rotating permanent magnet; (4) Add solution B to the micro-pipette and suspend it above the liquid tank of the liquid distributor; (5) Set the rotation speed of the permanent magnet to 600 rpm; (6) After the liquid distributor rotates stably for 1 minute to form a stable flow field in glycerol, gradually add 0.1 mL of solution B into the liquid tank of the liquid distributor through the micro-pipette; (7) Under the combined action of gravity, centrifugal force and surface tension, the added solution B is dispersed and discharged through the five inclined channels connected to the liquid distributor and enters the mixed solution. The magnetic control part stirs at the same time to promote the mixing of the two. Under the action of pH reduction and salting out, lysozyme crystals appear in the solution.

[0046] The differences between Examples 1, 2, and 3 are: (1) the frequencies of the three-dimensional AC magnetic fields used are different; in Example 1, it is 2Hz, in Example 2, it is 6Hz, and in Example 3, it is 8Hz. The difference in magnetic field frequency leads to differences in the final dispersion and mixing performance; (2) the magnetic material used in Example 3 is neodymium iron boron powder, which is different from the iron oxide powder used in Examples 1 and 2. The difference between Example 4 and Examples 1, 2, and 3 is the different way of introducing the rotating magnetic field. Examples 1, 2, and 3 are generated by passing AC power of different frequencies through a three-dimensional magnetic field generator, while Example 4 is generated by rotating a permanent magnet. The difference between Example 5 and other examples is that Example 5 designs a curved triangular liquid distributor and applies it to the liquid phase crystallization process.

[0047] It should be noted that the embodiments listed in this patent are individual embodiments implemented based on the principles, methods, structures, and shapes involved in this invention, and the technical features of this invention are not limited to the listed embodiments. Therefore, any equivalent changes made without inventive innovation based on the principles, methods, structures, and shapes disclosed in this invention should be included within the scope of protection claimed by this patent.

Claims

1. A method for simultaneous mixing of liquids by magnetically driven enhanced liquid addition, characterized in that, Includes the following steps: (1) Design of liquid distributor: The main structure of the liquid distributor is a curved polygon with a certain thickness; the curved polygon is a rotationally symmetric structure containing 2-8 corners; the liquid distributor is divided into a dispersion section and a magnetic control section, the dispersion section includes a liquid tank and flow channels; the flow channels are inclined flow channels; the bottom of the liquid tank is connected to all flow channels; the liquid tank is circular and located at the center of the dispersion section; the inclined flow channels are opened on the curved polygon; (2) Manufacturing of liquid distributor: By 3D printing the dispersion part and the magnetron part, magnetic material is added into the groove, and then the dispersion part and the magnetron part are combined into one piece by ultraviolet light curing. (3) Dispersing the liquid: 1) Add the bulk liquid phase to the reaction vessel; 2) Place the liquid distributor in the reaction vessel, with the magnetron submerged in the bulk liquid phase and the dispersion section exposed above the surface of the bulk liquid phase; 3) Transfer the reaction vessel to the platform of the three-dimensional magnetic field generator; 4) After adding the liquid to be dispersed into the micropipette, suspend the micropipette above the corresponding liquid tank of the liquid distributor; 5) Turn on the magnetic field, and set the magnetic field strength and frequency; 6) After the liquid distributor has been rotating stably for a period of time and a stable flow field has been formed in the bulk liquid phase, the liquid to be dispersed is dripped into the liquid tank of the liquid distributor through a micro-syringe. 7) The added dispersed liquid is dispersed and discharged through the inclined flow channel connected to the liquid tank under the combined action of gravity, centrifugal force and surface tension, and enters the main liquid phase. At the same time, the magnetic control unit stirs to promote the mixing of the two phases.

2. The method for simultaneous mixing of liquids based on magnetically driven enhancement according to claim 1, characterized in that, The flow channel is inclined in the direction of decreasing height of the distribution section, with an inclination angle of 1°-30°, and the flow channel is distributed at one or more corners.

3. The method for simultaneous mixing of liquids based on magnetically driven enhancement according to claim 1, characterized in that, The magnetic control unit is located in a sealed groove at the bottom center of the dispersion unit, and the sealed groove is filled with magnetic material.

4. The method for simultaneous mixing of liquids based on magnetically driven enhancement according to claim 3, characterized in that, The magnetic material is one or a mixture of two or more of the following: iron oxide powder, neodymium iron boron powder, and chromium dioxide powder.

5. The method for simultaneous mixing of liquids based on magnetically driven enhancement according to claim 3, characterized in that, The magnetic field is a rotating magnetic field, generated by an alternating current supplied to a three-dimensional magnetic field generator or by the rotation of a permanent magnet. The magnetic field strength is 5 Gs-1000 Gs, and the frequency of the rotating magnetic field is 0-30 Hz.

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