CN109012445B - Automatic nano-bubble preparation device and preparation method thereof - Google Patents

Automatic nano-bubble preparation device and preparation method thereof Download PDF

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CN109012445B
CN109012445B CN201810874152.2A CN201810874152A CN109012445B CN 109012445 B CN109012445 B CN 109012445B CN 201810874152 A CN201810874152 A CN 201810874152A CN 109012445 B CN109012445 B CN 109012445B
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injector
reaction bottle
chuck
stepping motor
automatic
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CN109012445A (en
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杨芳
冯振强
顾宁
金娟
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Southeast University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/80—Mixing plants; Combinations of mixers
    • B01F33/81—Combinations of similar mixers, e.g. with rotary stirring devices in two or more receptacles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/20—Mixing gases with liquids
    • B01F23/23—Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids
    • B01F23/232—Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids using flow-mixing means for introducing the gases, e.g. baffles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/40—Mounting or supporting mixing devices or receptacles; Clamping or holding arrangements therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
    • B01F2101/48—Mixing water in water-taps with other ingredients, e.g. air, detergents or disinfectants

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  • Chemical Kinetics & Catalysis (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention discloses an automatic nanometer bubble preparation device and a preparation method thereof, wherein the preparation device comprises a box body, a control center, a motion unit, a temperature control unit, an air charging and discharging unit, a reaction bottle, a communicating pipe and an injector, the control center is arranged in the box body, the reaction bottle is connected with the injector through the communicating pipe, the motion unit comprises a stepping motor, an electric motion platform, an air cylinder, a top plug chuck, an injector chuck and a reaction bottle chuck, and the stepping motor is connected with the control center. The preparation method comprises the following steps: a. starting the device; b. exhausting and inflating; c. installing an injector and a reaction bottle; d. adjusting the temperature to a set temperature; e. setting a motion mode of a stepping motor; f. the stepping motor moves according to a set mode; g. and stopping the device. The invention utilizes the principle of hydrodynamic cavitation, and utilizes full-automatic equipment to generate nano bubbles through high-speed water flow repeatedly sprayed by an injector, thereby being capable of preparing nano bubbles wrapped by nano particles with adjustable concentration and uniform and controllable size in batches.

Description

Automatic nano-bubble preparation device and preparation method thereof
Technical Field
The invention belongs to the technical field of nanometer, and particularly relates to an automatic nanometer bubble preparation device and a preparation method thereof.
Background
Nanobubbles are tiny bubbles with a size of hundreds of nanometers and less in solution. According to numerous reports, nanobubbles in water have several properties:
(1) has strong stability: can be preserved for more than 10 days at normal temperature and normal pressure;
(2) has strong adsorption capacity: micro-nano bubbles are commonly used in industry to adsorb micro particles;
(3) has strong acoustic characteristics: the micro-nano bubbles are used as an ultrasonic contrast agent for clinical application.
The existing method for preparing the nano bubbles mainly comprises mechanical stirring, electrolysis, ultrasonic cavitation and the like. Mechanical stirring passes through the motor and drives the turbine rotation, cuts the rivers and forms nanometer bubble, has certain advantage on the nanometer bubble of preparation bulk volume, but because the sample is direct and the motor contact, probably by impurity pollution, it is lower to prepare nanometer bubble concentration moreover. The electrolysis process can be carried out in a small system, but since the bubbles are generated by electrolysis, this process is not feasible when producing special gas bubbles, such as sulfur hexafluoride bubbles. The ultrasonic cavitation also has the defects of low concentration of prepared bubbles, wide particle size distribution and the like. Particularly, the traditional emulsion method, ultrasonic cavitation method, micro-channel method and the like are still adopted in the current bubble preparation method carrying nano particles, bubbles prepared by the methods are in a micron scale, but reports on uniform and controllable nano-scale bubbles are not available.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects in the prior art, the invention aims to provide an automatic nano-bubble preparation device, and the invention also aims to provide a preparation method for preparing automatic nano-particle self-assembly nano-bubbles with uniform bubble size and controllable shape and quantity.
The technical scheme is as follows: the invention relates to an automatic nano-bubble preparation device, which comprises a box body, a control center, a motion unit, a temperature control unit, an air charging and exhausting unit, a reaction bottle, a communicating pipe and an injector, wherein the control center is arranged in the box body, the temperature control unit is respectively connected with the reaction bottle and the control center, the motion unit is fixedly connected with the box body, the reaction bottle is connected with the injector through the communicating pipe, the motion unit comprises a stepping motor, an electric motion platform, an air cylinder, a top plug chuck, an injector chuck and a reaction bottle chuck, the stepping motor is connected with the control center, the motion unit uses the stepping motor as power, and the stepping motor drives the top plug of the injector to move, so that nano-particles are self-assembled into a controllable nano-bubble structure, and the air cylinder is.
The control center comprises a serial port screen, a Micro Python core board, a serial port level conversion module and a stepping motor driver, according to the control principle of the stepping motor, the serial port screen sends an instruction to the Micro Python core board, the Micro Python core board generates pulse waves with different frequencies to the stepping motor driver, and the control of the movement distance of the stepping motor is realized through the number of generated pulses. The temperature control unit is a TEC temperature controller, reads the temperature in real time, and sets the target temperature by sending data to the control unit. The top plug chuck is connected with a sliding groove of the electric motion platform in a sliding mode through a sliding block at the bottom. The exhaust unit comprises an air tank, an air pump, an electromagnetic valve and a rubber tube. The communicating pipe is provided with three branch pipes and an intermediate body, and the branch pipes are respectively provided with a valve.
The invention relates to a preparation method of automatic nanoparticle self-assembly nanobubbles, which comprises the following steps:
a. starting an automatic nano-bubble preparation device;
b. discharging air in the injector and the reaction bottle, filling gas which does not chemically react with water and is insoluble in water into the injector and the communicating pipe, wherein the gas can be sulfur hexafluoride, perfluorocarbon gas, nitric oxide, hydrogen sulfide, carbon monoxide, oxygen, hydrogen or helium, deionized water and nanoparticles are arranged in the reaction bottle, and the nanoparticles are superparamagnetic iron oxide nanoparticles, gold nanoparticles or silver nanoparticles;
c. installing an injector and a reaction bottle, clamping a top plug of the injector by using a top plug chuck, clamping a bottle body of the injector by using an injector chuck, clamping the bottle body of the reaction bottle by using a reaction bottle chuck, and enabling a needle head of the injector to be above the liquid level;
d. adjusting the temperature to a set temperature of 1-50 ℃;
e. setting the motion mode of the stepping motor, namely setting the speed of the stepping motor to be 10-30mm/s, the motion distance to be 1-200mm and the reciprocating motion times to be 2-1000;
f. the stepping motor moves according to a set mode, the top plug moves downwards to reduce the volume of the gas, and then moves upwards to make part of water enter the communicating pipe and repeatedly and circularly compress at a constant speed of 10-30 mm/s;
g. and stopping the device.
Has the advantages that: compared with the prior art, the invention has the following remarkable characteristics: the invention utilizes the principle of hydrodynamic cavitation, and utilizes full-automatic equipment to generate nano bubbles through high-speed water flow repeatedly sprayed by an injector, so that a nano bubble material wrapped by biomedical nano particles with adjustable concentration and uniform and controllable size can be prepared in batches; the full-automatic mechanical operation of the invention is beneficial to saving manpower and time and reducing the contingency caused by manual operation; the preparation method is favorable for improving the ultrasonic asymmetric vibration of the bubbles under the condition of not enhancing the excitation signal, and can be used for enhancing ultrasonic targeted development.
Drawings
Fig. 1 is a perspective view of an automated nanobubble preparation device of the present invention.
FIG. 2 is a partially enlarged view of the reaction flask and syringe according to the present invention.
Fig. 3 is a schematic view of the structure of the motion unit of the present invention.
FIG. 4 is a graph showing the particle size distribution of a sample obtained in example 5 of the present invention.
FIG. 5 is a scanning electron microscope photograph of a sample prepared in example 5 of the present invention.
FIG. 6 is a transmission electron microscope photograph of a sample prepared in example 6 of the present invention.
Detailed Description
As shown in fig. 1, the automatic nano-bubble preparation device comprises a box body 1, a control center 2, a motion unit 3, a temperature control unit, an air charging and discharging unit, a reaction bottle 4, a communicating pipe 5 and an injector 6, wherein the control center 2 is arranged at one side of the box body 1, a plurality of groups of motion units 3 are fixed on the box body 1, the device can realize temperature control, automatic air charging and discharging and automatic nano-bubble preparation.
Referring to fig. 2, the reaction flask 4 is connected with the injector 6 through the communicating tube 5, the communicating tube 5 has three branch tubes and an intermediate body, the branch tubes are respectively connected with the valves 14, the needle 16 of the injector 6 is inserted into the reaction flask 4, and the reaction flask 4 is sealed by an aluminum cap and a rubber plug. The valve 14 may be replaced by a rubber stopper to perform the sealing function.
As shown in fig. 3, the moving unit 3 includes a stepping motor 7, an electric moving platform 8, an air cylinder 9, a plunger chuck 10, a syringe chuck 11 and a reaction vial chuck 12, the moving mode of the stepping motor 7 is controlled by the control center 2, the electric moving platform 8 drives a piston to move up and down, the air cylinder 9 is used for driving the reaction vial chuck 12 to move up and down, the air cylinder 9 is preferably a linear moving air cylinder 9, the plunger chuck 10 is used for clamping a plunger 15 of the syringe 6, the syringe chuck 11 is used for clamping a body of the syringe 6, and the reaction vial chuck 12 is used for clamping a body of the reaction vial 4.
The superparamagnetic iron oxide nanoparticles are ferric oxide nanoparticles or ferroferric oxide nanoparticles.
Preparation method example 1
A method for preparing automatic nanoparticle self-assembly nanobubbles comprises the following steps:
1. starting an automatic nano-bubble preparation device;
2. discharging the air in the injector 6 and the reaction bottle 4, filling perfluorocarbon gas into the injector 6 and the communicating pipe 5, and filling 2ml of deionized water and 2 mul of superparamagnetic ferroferric oxide nanoparticles into the reaction bottle 4;
3. installing the syringe 6 and the reaction bottle 4, clamping the top plug 15 of the syringe 6 by using a top plug chuck 10, clamping the bottle body of the syringe 6 by using a syringe chuck 11, clamping the bottle body of the reaction bottle 4 by using a reaction bottle chuck 12, and enabling the needle head 16 of the syringe 6 to be above the liquid level to form a closed system, wherein the total volume V of air is0＝4.5mL；
4. Adjusting the temperature to 1 ℃;
5. setting a motion mode of the stepping motor 7, namely setting the speed of the stepping motor 7 to be 15mm/s, the motion distance to be 1mm and the reciprocating motion times to be 2 times;
6. the stepping motor 7 moves according to a set mode, and the top plug 15 moves downwards to reduce the volume of the gas to V1When the pressure is 1.5mL and the pressure is 0.3MPa, the gas moves upwards to make part of water enter the communicating pipe 5, and the total volume of the gas is returned to V2Mixing gas and water under certain pressure at constant speed of 15mm/s 2.5mL, and repeatedly compressing for 2 times;
7. and stopping the device.
Preparation method example 2
A method for preparing automatic nanoparticle self-assembly nanobubbles comprises the following steps:
1. starting an automatic nano-bubble preparation device;
2. discharging the air in the injector 6 and the reaction bottle 4, filling nitric oxide gas into the injector 6 and the communicating pipe 5, and filling 2ml of deionized water and 2 mu l of ferric oxide nanoparticles in the reaction bottle 4;
3. the syringe 6 and the reaction flask 4 are assembled, the plunger 15 of the syringe 6 is clamped by the plunger chuck 10, and the injection is carried outThe syringe 6 is clamped by the device chuck 11, the reaction bottle 4 is clamped by the reaction bottle chuck 12, the needle 16 of the syringe 6 is above the liquid level to form a closed system, and the total volume V of air0＝4.5mL；
4. Adjusting the temperature to 50 ℃;
5. setting a motion mode of the stepping motor 7, namely setting the speed of the stepping motor 7 to be 25mm/s, the motion distance to be 200mm and the reciprocating motion times to be 1000;
6. the stepping motor 7 moves according to a set mode, and the top plug 15 moves downwards to reduce the volume of the gas to V1When the pressure is 1.5mL and the pressure is 0.3MPa, the gas moves upwards to make part of water enter the communicating pipe 5, and the total volume of the gas is returned to V2Mixing gas and water under certain pressure at constant speed of 25mm/s 2.5mL, and repeatedly compressing for 1000 times;
7. and stopping the device.
Preparation method example 3
A method for preparing automatic nanoparticle self-assembly nanobubbles comprises the following steps:
1. starting an automatic nano-bubble preparation device;
2. exhausting the air in the injector 6 and the reaction bottle 4, filling hydrogen sulfide gas into the injector 6 and the communicating pipe 5, and filling 2ml of deionized water and 2 mul of silver nanoparticles in the reaction bottle 4;
3. installing the syringe 6 and the reaction bottle 4, clamping the top plug 15 of the syringe 6 by using a top plug chuck 10, clamping the bottle body of the syringe 6 by using a syringe chuck 11, clamping the bottle body of the reaction bottle 4 by using a reaction bottle chuck 12, and enabling the needle head 16 of the syringe 6 to be above the liquid level to form a closed system, wherein the total volume V of air is0＝4.5mL；
4. Adjusting the temperature to 25 ℃;
5. setting a motion mode of the stepping motor 7, namely setting the speed of the stepping motor 7 to be 20mm/s, the motion distance to be 100mm and the reciprocating motion times to be 500 times;
6. the stepping motor 7 moves according to a set mode, and the top plug 15 moves downwards to reduce the volume of the gas to V11.5mL, at a pressure of 0.3MPa, and moving upward to introduce part of water into the connecting pipePipe 5, the total volume of gas is returned to V2Mixing gas and water under certain pressure at constant speed of 20mm/s 2.5mL, and repeatedly compressing for 500 times;
7. and stopping the device.
Preparation method example 4
A method for preparing automatic nanoparticle self-assembly nanobubbles comprises the following steps:
1. starting an automatic nano-bubble preparation device;
2. discharging the air in the injector 6 and the reaction bottle 4, filling carbon monoxide gas into the injector 6 and the communicating pipe 5, and filling 2ml of deionized water and 2 mul of gold nanoparticles in the reaction bottle 4;
3. installing the syringe 6 and the reaction bottle 4, clamping the top plug 15 of the syringe 6 by using a top plug chuck 10, clamping the bottle body of the syringe 6 by using a syringe chuck 11, clamping the bottle body of the reaction bottle 4 by using a reaction bottle chuck 12, and enabling the needle head 16 of the syringe 6 to be above the liquid level to form a closed system, wherein the total volume V of air is0＝4.5mL；
4. Adjusting the temperature to 10 ℃;
5. setting a motion mode of the stepping motor 7, namely setting the speed of the stepping motor 7 to be 13mm/s, the motion distance to be 40mm and the reciprocating motion times to be 700 times;
6. the stepping motor 7 moves according to a set mode, and the top plug 15 moves downwards to reduce the volume of the gas to V1When the pressure is 1.5mL and the pressure is 0.3MPa, the gas moves upwards to make part of water enter the communicating pipe 5, and the total volume of the gas is returned to V2Mixing gas and water under certain pressure at constant speed of 13mm/s 2.5mL, and repeatedly compressing for 800 times;
7. and stopping the device.
The carbon monoxide gas may be replaced by a gas that does not chemically react with water and is hardly soluble in water, such as oxygen gas, hydrogen gas, or helium gas.
Preparation method example 5
A method for preparing automatic nanoparticle self-assembly nanobubbles comprises the following steps:
1. starting an automatic nano-bubble preparation device;
2. discharging the air in the injector 6 and the reaction bottle 4, filling sulfur hexafluoride gas into the injector 6 and the communicating pipe 5, and filling 2ml of deionized water and 2 mul of superparamagnetic ferroferric oxide nanoparticles into the reaction bottle 4;
3. installing the syringe 6 and the reaction bottle 4, clamping the top plug 15 of the syringe 6 by using a top plug chuck 10, clamping the bottle body of the syringe 6 by using a syringe chuck 11, clamping the bottle body of the reaction bottle 4 by using a reaction bottle chuck 12, and enabling the needle head 16 of the syringe 6 to be above the liquid level to form a closed system, wherein the total volume V of air is0＝4.5mL；
4. Adjusting the temperature to 40 ℃;
5. setting a motion mode of the stepping motor 7, namely setting the speed of the stepping motor 7 to be 30mm/s, the motion distance to be 50mm and the reciprocating motion times to be 100 times;
6. the stepping motor 7 moves according to a set mode, and the top plug 15 moves downwards to reduce the volume of the gas to V1When the pressure is 1.5mL and the pressure is 0.3MPa, the gas moves upwards to make part of water enter the communicating pipe 5, and the total volume of the gas is returned to V2Mixing gas and water under certain pressure at constant speed of 30mm/s 2.5mL, and repeatedly compressing for 100 times;
7. and stopping the device.
FIG. 4 is a particle size distribution diagram of the sample prepared in example 5, which is measured by a Malvern particle size analyzer, and it can be seen from the graph that the average particle size of the sample is 100-300nm, the polydispersity PDI is 0.2-0.4, the PDI (dispersion coefficient) is 0.28, the particle size of the representative sample is uniform, the dispersibility is good, and the Z-average (average particle size) is 237 nm. FIG. 5 shows the shape of the sample under the scanning electron microscope, and the white spheres are the structural shapes of the magnetic nanobubbles.
Preparation method example 6
A method for preparing automatic nanoparticle self-assembly nanobubbles comprises the following steps:
1. starting an automatic nano-bubble preparation device;
2. exhausting the air in the injector 6 and the reaction bottle 4, filling sulfur hexafluoride gas into the injector 6 and the communicating pipe 5, and filling 2ml of deionized water and 2 mul of gold nanoparticles in the reaction bottle 4;
3. installing the syringe 6 and the reaction bottle 4, clamping the top plug 15 of the syringe 6 by using a top plug chuck 10, clamping the bottle body of the syringe 6 by using a syringe chuck 11, clamping the bottle body of the reaction bottle 4 by using a reaction bottle chuck 12, and enabling the needle head 16 of the syringe 6 to be above the liquid level to form a closed system, wherein the total volume V of air is0＝4.5mL；
4. Adjusting the temperature to 15 ℃;
5. setting a motion mode of the stepping motor 7, namely setting the speed of the stepping motor 7 to be 10mm/s, the motion distance to be 120mm and the reciprocating motion times to be 100 times;
6. the stepping motor 7 moves according to a set mode, and the top plug 15 moves downwards to reduce the volume of the gas to V1When the pressure is 1.5mL and the pressure is 0.3MPa, the gas moves upwards to make part of water enter the communicating pipe 5, and the total volume of the gas is returned to V2Mixing gas and water under certain pressure at constant speed of 10mm/s 2.5mL, and repeatedly compressing for 100 times;
7. and stopping the device.
FIG. 6 is a TEM image of a sample prepared in example 6 of the present invention, from which it can be seen that gold nanoparticles are self-assembled into a spherical bubble structure.

Claims (9)

1. A method for preparing automatic nanoparticle self-assembly nanobubbles is characterized by comprising the following steps:
(a) starting an automatic nano-bubble preparation device;
(b) exhausting the air in the injector (6) and the reaction bottle (4), filling gas which does not chemically react with water and is insoluble in water into the injector (6) and the communicating pipe (5), and filling deionized water and nano particles in the reaction bottle (4);
(c) installing an injector (6) and a reaction bottle (4), clamping a top plug (15) of the injector (6) by a top plug chuck (10), clamping a bottle body of the injector (6) by an injector chuck (11), clamping the bottle body of the reaction bottle (4) by a reaction bottle chuck (12), and keeping a needle head (16) of the injector (6) below the liquid level;
(d) adjusting the temperature to a set temperature of 1-50 ℃;
(e) setting a motion mode of the stepping motor (7), namely setting the speed of the stepping motor (7) to be 10-30mm/s, the motion distance to be 1-200mm and the reciprocating motion times to be 2-1000;
(f) the stepping motor (7) moves according to a set mode, the top plug (15) moves downwards to reduce the volume of the gas, and then moves upwards to make part of water enter the communicating pipe (5) and repeatedly and circularly compress at a constant speed;
(g) a stopping device;
the automatic nano-bubble preparation device comprises a box body (1), a control center (2), a motion unit (3), a temperature control unit, an air charging and discharging unit, a reaction bottle (4), a communicating pipe (5) and an injector (6), the control center (2) is arranged in the box body (1), the temperature control unit is respectively connected with the reaction bottle (4) and the control center (2), the moving unit (3) is fixedly connected with the box body (1), the reaction bottle (4) is connected with the injector (6) through a communicating pipe (5), the moving unit (3) comprises a stepping motor (7), an electric moving platform (8), a cylinder (9), a top plug chuck (10), an injector chuck (11) and a reaction bottle chuck (12), the stepping motor (7) is connected with the control center (2), and the air cylinder (9) is used for driving the reaction bottle chuck (12) to lift.
2. The method of claim 1, wherein the automated nanoparticle self-assembly nanobubble preparation comprises: control center (2) include serial ports screen, Micro Python core plate, serial ports level conversion module and step motor (7) driver, serial ports screen send instruction gives Micro Python core plate, generates the pulse wave of different frequencies and gives step motor (7) driver.
3. The method of claim 1, wherein the automated nanoparticle self-assembly nanobubble preparation comprises: the temperature control unit is a TEC temperature controller.
4. The method of claim 1, wherein the automated nanoparticle self-assembly nanobubble preparation comprises: the top plug chuck (10) is in sliding connection with a sliding groove of the electric motion platform (8) through a sliding block (13) at the bottom.
5. The method of claim 1, wherein the automated nanoparticle self-assembly nanobubble preparation comprises: the exhaust unit comprises an air tank, an air pump, an electromagnetic valve and a rubber tube.
6. The method of claim 1, wherein the automated nanoparticle self-assembly nanobubble preparation comprises: the communicating pipe (5) is provided with three branch pipes and an intermediate body, and the branch pipes are respectively provided with a valve (14).
7. The method for preparing the automatic nanoparticle self-assembly nanobubbles of claim 1, wherein: the gas in the step (b) is sulfur hexafluoride, perfluorocarbon gas, nitric oxide, hydrogen sulfide, carbon monoxide, oxygen, hydrogen or helium.
8. The method for preparing the automatic nanoparticle self-assembly nanobubbles of claim 1, wherein: the nanoparticles in the step (b) are superparamagnetic iron oxide nanoparticles, gold nanoparticles or silver nanoparticles.
9. The method for preparing the automatic nanoparticle self-assembly nanobubbles of claim 1, wherein: the constant speed in the step (f) is 10-30 mm/s.
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