Device and method for synthesizing inorganic nanoparticles through magnetic vortex energy transfer continuous flow
Through magnetic vortex technology combined with flow synthesis technology, the problems of medium and low yields, uneven particle size and complex production of inorganic nanoparticle synthesis are solved, and efficient, stable and controllable nanoparticle synthesis is achieved, which is suitable for industrial production.
Patent Information
- Application Number
- CN202510368782.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-27
- Publication Date
- 2025-05-27
AI Technical Summary
The existing inorganic nanoparticle synthesis methods have problems such as low yield, uneven particle size, complex production process, and difficult to achieve industrial production and reaction conditions.
The continuous flow synthesis of inorganic nanoparticles is achieved through magnetic vortex energy transfer using magnetic vortex energy. The device includes a nanoparticle generator, a reaction liquid delivery system, a backpressure valve, a controller, a product cooler and a product collector. By precisely controlling the reaction temperature and pressure, the synthesis of inorganic nanoparticles with high crystallinity and narrow particle size distribution can be achieved.
It realizes efficient, stable and controllable synthesis of inorganic nanoparticles, significantly improves yield and product quality, and is suitable for industrial production.
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Figure CN120037858A_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the fields of nanotechnology and materials science, and particularly relates to an apparatus and method for continuously flowing synthesis of inorganic nanoparticles through magnetic vortex energy transfer. Background Art
[0002] Nanoparticles (NPs) are a class of materials characterized by a nanoscale size (1 - 100 nanometers). Due to their unique size effect, surface effect, quantum effect, and interface effect, they have become the focus of research in fields such as materials science, chemistry, biomedicine, and environmental engineering in recent years. The high specific surface area and tunable physicochemical properties of nanoparticles make them show great application potential in catalysts, drug delivery, energy storage, biosensing, optical devices, and pollution control. However, although inorganic nanoparticles have significant application potential, existing synthesis methods still face many challenges and technical bottlenecks in practical applications. The specific problems are as follows:
[0003] 1. Low yield problem: Traditional inorganic nanoparticle synthesis methods such as co - precipitation method, thermal decomposition method, and solvothermal method are mostly batch reactions. This reaction mode has limited production capacity and is difficult to achieve large - scale continuous production. Batch reactions require cleaning the reactor, refilling materials, and adjusting reaction conditions after each reaction, resulting in a long cycle for each reaction and low yield. This low - yield production method cannot meet the requirements of large - scale industrial production.
[0004] 2. Particle size non - uniformity problem: The physicochemical properties of inorganic nanoparticles largely depend on their particle size. Inorganic nanoparticles obtained by traditional synthesis methods often have a wide particle size distribution, which seriously affects their application effects and reliability.
[0005] 3. Complex production process problem: Existing synthesis methods usually require complex operation steps and harsh reaction conditions. For example, thermal decomposition method and solvothermal method often require high temperature, high pressure, and inert atmosphere to ensure the smooth progress of the reaction. These conditions not only increase the complexity of equipment and operation but also raise production costs. In addition, operators need to have a high technical level to ensure the safety of the production process and product quality.
[0006] 4. Difficulty in industrial production problem: The scale of batch reactors is limited and difficult to meet the requirements of industrial production. During the process of expanding production scale, traditional synthesis methods often have problems such as non - uniform particle size and decreased performance. These problems are not obvious in laboratory preparation but will significantly affect the quality and consistency of products during industrial scale - up production. Therefore, existing batch reactors are difficult to meet the requirements of industrial large - scale production of high - quality nanoparticles.
[0007] 5. Problem of difficult precise control of reaction conditions: In traditional synthesis devices, the heating method is mostly external heating, that is, heat is conducted to the reactants by heating the outer wall of the reactor. This heating method has problems such as uneven heating, resulting in difficult precise control of reaction conditions. For example, in the thermal decomposition method, a slight fluctuation in the reaction temperature may significantly affect the size and morphology of nanoparticles. In addition, the response time of the external heating method is long, and it is difficult to achieve rapid and precise temperature control, which is a huge problem faced in the preparation of high-quality nanoparticles using traditional synthesis devices.
[0008] The synthesis method based on magnetic vortex can solve the above problems and can achieve rapid and efficient synthesis of nanomaterials under relatively mild conditions. Specifically, the magnetic vortex technology induces eddy currents in conductive materials using electromagnetic fields and converts electrical energy into heat energy through resistive heating. This heating method has the advantages of fast heating speed, precise temperature control, and good uniformity, and is very suitable for the synthesis of nanoparticles.
[0009] The specific advantages are as follows:
[0010] 1. Fast heating speed: The magnetic vortex can heat the reactants to the required temperature in a short time, significantly shortening the reaction time, with excellent responsiveness, which is beneficial to improving production efficiency.
[0011] 2. Precise temperature control: The magnetic vortex can achieve precise control of the heating temperature to ensure that the reaction proceeds under stable and controllable temperature conditions.
[0012] 3. Good heating uniformity: The magnetic vortex generates eddy currents inside the conductive material, making the heat evenly distributed and avoiding the heat gradient problem existing in the external heating method.
[0013] Based on the above advantages, the application prospect of the magnetic vortex heating technology in the synthesis of nanomaterials is very broad. However, there is currently no magnetic vortex synthesis device for the continuous flow synthesis of inorganic nanoparticles on the market. The existing magnetic vortex synthesis devices are mostly intermittent reactors for laboratory use, and it is difficult to achieve continuous production and industrial application. Summary of the Invention
[0014] Aiming at the problems existing in the prior art, the present invention provides a device and method for continuously flowing and synthesizing inorganic nanoparticles through magnetic vortex energy transfer. By combining magnetic vortex technology with flow synthesis technology, inorganic nanoparticles with high crystallinity and narrow particle size distribution are prepared to achieve stable and repeatable preparation of inorganic nanoparticles, and macroscale preparation of nanoparticles is achieved through continuous sampling.
[0015] To solve the above technical problems, the present invention is realized through the following technical solutions:
[0016] An apparatus for continuously synthesizing inorganic nanoparticles through magnetic vortex energy transfer, comprising at least a nanoparticle generator, a reaction liquid delivery system, a back pressure valve, and a controller. According to process requirements, it may also include a product cooler and a product collector; wherein,
[0017] The reaction liquid delivery system is used to deliver the reaction liquid containing the metal salt precursor to the nanoparticle generator at a certain flow rate for reaction, and then deliver the generated inorganic nanoparticles to the product collector through the product cooler at a certain flow rate;
[0018] The nanoparticle generator is used to heat the reaction liquid flowing through it by means of magnetic vortex energy transfer, so that the reactants undergo a chemical reaction under the action of the magnetic vortex to generate inorganic nanoparticles;
[0019] The back pressure valve is connected between the product cooler and the product collector, and is used to control the pressure required for the reaction system;
[0020] The controller is used to monitor the working states of the nanoparticle generator and the reaction liquid delivery system to ensure that the reaction liquid in the nanoparticle generator reacts under preset conditions;
[0021] The product cooler is used to cool the generated inorganic nanoparticles;
[0022] The product collector is used to collect the cooled inorganic nanoparticles.
[0023] Furthermore, the nanoparticle generator includes at least one magnetic vortex reactor unit, at least one temperature feedback unit, and at least one pressure feedback unit;
[0024] Each magnetic vortex reactor unit is composed of a reaction pipeline and a heater; the reaction pipeline is a millimeter fluid system, and the pipe diameter size of the reaction pipeline is 0.05 - 20 mm; one end of the reaction pipeline is communicated with the reaction liquid delivery system, and the other end of the reaction pipeline is communicated with the product cooler; the heater is signal-connected to the controller to achieve precise control of the heating temperature; the heater generates a magnetic vortex for the reaction pipeline by controlling the magnetic field intensity of the alternating current coil, so that the reaction liquid flowing through the reaction pipeline is in a preset condition under the electromagnetic action, and thus reacts to generate inorganic nanoparticles;
[0025] When the nanoparticle generator contains multiple series-connected nanoparticle generator units, each nanoparticle generator unit adopts a modular design, and adjacent two sections of the reaction pipelines are connected through corresponding connecting pipelines;
[0026] The temperature feedback unit is connected to the controller. Each temperature feedback unit is responsible for detecting the temperature inside its corresponding reaction pipe and feeding back the temperature signal to the controller, so that the controller can adjust the temperature of the reaction liquid inside the corresponding reaction pipe according to the received temperature signal;
[0027] The pressure feedback unit is connected to the controller. Each pressure feedback unit is responsible for detecting the pressure inside its corresponding reaction pipe and feeding back the pressure signal to the controller, so that the controller can adjust the flow rate of the reaction liquid delivery and the reaction pressure inside the corresponding reaction pipe according to the received pressure signal;
[0028] Through the precise control of the reaction temperature and reaction pressure in the nanoparticle generator, the flow synthesis of inorganic nanoparticles with more uniform sizes is realized.
[0029] Furthermore, the temperature range of the reaction pipe under the regulation of the heater is 0 to 500 °C.
[0030] Furthermore, the temperature feedback unit is a temperature sensor.
[0031] Furthermore, the pressure feedback unit is a pressure sensor.
[0032] Furthermore, the material of the reaction pipe is a metallic material, including one or more of carbon steel, Hastelloy, 304 stainless steel, 316 stainless steel, 316L stainless steel, chrome molybdenum alloy steel, low alloy high strength steel, pure copper, brass, Inconel alloy, pure titanium, titanium alloy, hot-dip galvanized steel, pure lead, duplex stainless steel, super stainless steel.
[0033] Furthermore, the reaction liquid delivery system includes a reaction liquid storage tank, a sampling pipe, multiple delivery pipes, a sampling valve, and a sampling pump; the reaction liquid storage tank is used to store the prepared reaction liquid containing the metal salt precursor; the reaction liquid storage tank is connected to the nanoparticle generator through the sampling pipe, the nanoparticle generator is connected to the product cooler through the corresponding delivery pipe, the product cooler is connected to the product collector through the corresponding delivery pipe, the sampling valve and the sampling pump are arranged on the sampling pipe and are both connected to the controller. Under the control of the controller, the sampling valve and the sampling pump regulate the fluid flow rate and residence time inside the reaction pipe; the pipe diameter size range of the delivery pipe is between 0.05 and 20 mm.
[0034] Further, the reaction solution delivery system includes multiple reaction solution reservoirs, multiple sampling pipes, multiple delivery pipes, at least one reagent mixer, multiple sampling valves, and multiple sampling pumps; each of the reaction solution reservoirs is respectively used to independently store the reagent raw materials required for preparing the reaction solution containing the metal salt precursor; the reagent mixer is used to mix the reagent raw materials delivered from each of the reaction solution reservoirs, so as to prepare a reaction solution containing the metal salt precursor; the reagent mixer is respectively connected to each of the reaction solution reservoirs through the corresponding sampling pipes, the reagent mixer is connected to the nanoparticle generator through the corresponding delivery pipe, the nanoparticle generator is connected to the product cooler through the corresponding delivery pipe, and the product cooler is connected to the product collector through the corresponding delivery pipe; a set of corresponding sampling valves and sampling pumps are arranged on each sampling pipe, and each set of sampling valves and sampling pumps is connected to the controller. Under the control of the controller, each set of sampling valves and sampling pumps regulates the fluid flow rate and residence time in the reaction pipe where they are located; the diameters of the sampling pipes and the delivery pipes range from 0.05 to 20 mm.
[0035] Further, the sampling valve is a flow controller.
[0036] Further, the sampling pump is a metering pump.
[0037] Further, the reagent mixer is a T-shaped, Y-shaped or static mixer.
[0038] Further, the product cooler is an air cooling device or a liquid cooling device.
[0039] Further, the controller is a computer, an industrial control computer or a microcontroller.
[0040] A method for continuously synthesizing inorganic nanoparticles by magnetic vortex energy transfer, which is realized by using the above-mentioned device for continuously synthesizing inorganic nanoparticles by magnetic vortex energy transfer, includes the following steps:
[0041] Step 1) Under the control of the controller, the sampling valve and the sampling pump deliver the prepared reaction solution from the reaction solution reservoir into the nanoparticle generator; in the nanoparticle generator, the heater makes the reaction solution flowing through the reaction pipe in a high-temperature state under the action of the magnetic vortex, so as to generate inorganic nanoparticles;
[0042] Step 2) Driven by the sampling pump, the inorganic nanoparticles generated by the reaction enter the product cooler with the fluid for cooling;
[0043] Step 3) Driven by the injection pump, the cooled inorganic nanoparticles enter the product collector along with the fluid. Further, in Step 1, the flow rate of the reaction solution is controlled at 0.02 - 1000 mL / min, preferably 0.1 - 500 mL / min.
[0044] Further, in Step 1, the reaction temperature is controlled at 120 - 500 °C, preferably 180 - 300 °C.
[0045] Further, in Step 1, the reaction pressure is controlled at 1 - 300 atmospheres, preferably 3 - 100 atmospheres.
[0046] Further, in Step 1, the residence time of the reaction solution in the reaction pipeline is controlled at 0.01 - 60 min.
[0047] Further, in Step 1, during the heating process, the temperature feedback unit and the pressure feedback unit respectively monitor the reaction temperature and the reaction pressure in the reaction pipeline, and regulate the heating temperature of the reaction pipeline and the pressure of the back pressure valve according to the temperature signal and the pressure signal to ensure that the reaction solution in the reaction pipeline is always under the preset conditions.
[0048] An inorganic nanoparticle prepared by using the device for continuously synthesizing inorganic nanoparticles through magnetic vortex energy transfer as described above and the method for continuously synthesizing inorganic nanoparticles through magnetic vortex energy transfer as described above.
[0049] The inorganic nanoparticle is a transition metal and its oxide, a lanthanide rare earth metal oxide, a transition metal or a rare earth metal doped magnetic oxide. More preferably, it is an oxide of iron, cobalt, nickel, manganese or iron / cobalt / nickel / gadolinium / terbium / dysprosium / holmium / erbium / thulium.
[0050] Further, the particle size of the inorganic nanoparticle is 1 - 100 nm.
[0051] Further, the surface of the inorganic nanoparticle is modified with one or more of small molecule amines, small molecule carboxylic acids, small molecule alcohols and small molecule phosphines with alkyl chains. For the small molecule amines, small molecule carboxylic acids, small molecule alcohols and small molecule phosphines with alkyl chains, the number of CH 2 units in the alkyl chain is 4 - 24, preferably 12 - 18, such as oleylamine, dodecylamine, oleic acid, 1,2-dodecanediol, octadecanol, etc.
[0052] Compared with the prior art, the beneficial effects of the present invention are:
[0053] The present invention uses a magnetic vortex continuous flow synthesis system to prepare inorganic nanoparticles, controlling the pressure and temperature to make the obtained inorganic nanoparticle products have high crystallinity, narrow particle size distribution and adjustable; the magnetic vortex continuous flow synthesis system of the present invention can be used to realize the automated synthesis of high-quality inorganic nanoparticles, with good stability and repeatability in product production, and small differences between batches, which is conducive to realizing the large-scale preparation of high-quality nanoparticles.
[0054] The above description is only an overview of the technical solution of the present invention. In order to be able to understand the technical means of the invention more clearly and to be implemented in accordance with the content of the specification, the following describes in detail with reference to the preferred embodiments of the present invention and the accompanying drawings. The specific implementation manners of the present invention are given in detail by the following embodiments and their accompanying drawings. BRIEF DESCRIPTION OF THE DRAWINGS
[0055] The drawings described herein are used to provide a further understanding of the present invention, and constitute a part of this application. The schematic embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. In the drawings:
[0056] Figure 1 It is a schematic diagram of the magnetic vortex continuous flow synthesis device in Embodiment 1 of the present invention.
[0057] Figure 2 It is a schematic diagram of the hybrid heating continuous flow synthesis device in Embodiment 2 of the present invention.
[0058] Figure 3 It is a schematic diagram of the multi-combination magnetic vortex continuous flow synthesis device in Embodiment 3 of the present invention.
[0059] Figure 4 It is a schematic diagram of the multi-injection channel magnetic vortex continuous flow synthesis device in Embodiment 4 of the present invention.
[0060] Figure 5 It is the transmission electron microscope photograph (A) and the particle size distribution histogram (B) of the magnetic Fe 3 O 4 nanoparticles obtained in Example 7-1 of the present invention.
[0061] Figure 6 It is the transmission electron microscope photograph (A) and the particle size distribution histogram (B) of the magnetic Fe 3 O 4 nanoparticles obtained in Example 7-2 of the present invention.
[0062] Figure 7 It is the transmission electron microscope photograph (A) and the particle size distribution histogram (B) of the magnetic Fe 3 O 4 nanoparticle hysteresis loop obtained in Example 7-2 of the present invention. DETAILED DESCRIPTION OF THE INVENTION
[0063] The preferred embodiments of the present invention will be described in detail below in conjunction with the accompanying drawings, so as to more clearly understand the purpose, features and advantages of the invention. It should be understood that the embodiments shown in the drawings are not limitations on the scope of the present invention, but only to illustrate the essential spirit of the technical solution of the present invention.
[0064] In the following description, certain specific details are set forth in order to provide a thorough understanding of the various disclosed embodiments. However, those skilled in the relevant art will recognize that the embodiments may be practiced without one or more of these specific details. In other instances, well-known devices, structures, and techniques associated with the present application may not be shown or described in detail so as not to unnecessarily obscure the description of the embodiments.
[0065] Unless the context requires otherwise, throughout the specification and claims, the words "comprising" and its variants, such as "comprises" and "having", should be understood in an open, inclusive sense, i.e., construed to mean "including, but not limited to".
[0066] References throughout the specification to "one embodiment" or "an embodiment" mean that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment. Thus, the appearances of "in one embodiment" or "in an embodiment" throughout the specification need not all refer to the same embodiment. Additionally, the particular features, structures, or characteristics may be combined in any manner in one or more embodiments.
[0067] As used in this specification and the appended claims, the singular forms "a" and "the" include plural referents unless the context clearly dictates otherwise. It should be noted that the term "or" is generally used in its inclusive sense of "and / or" unless the context clearly dictates otherwise.
[0068] Furthermore, the technical features involved in the different embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other. Unless otherwise specified, the reagents and materials used in the present invention are all commercially available.
[0069] Example 1 Magnetic Vortex Continuous Flow Synthesis Device:
[0070] See Figure 1 As shown, the magnetic vortex continuous flow synthesis device of this embodiment includes a nanoparticle generator, a product cooler 2, a product collector 3, a reaction liquid delivery system, a back pressure valve 1, and a controller.
[0071] The reaction liquid delivery system is used to deliver the reaction liquid containing the metal salt precursor to the nanoparticle generator at a certain flow rate for reaction, and then deliver the inorganic nanoparticles generated by the reaction to the product collector 3 at a certain flow rate through the product cooler 2. The reaction liquid delivery system includes a reaction liquid storage tank 7, a sampling pipeline, multiple delivery pipelines, a sampling valve 8, and a sampling pump 9. The reaction liquid storage tank 7 is used to store the prepared reaction liquid containing the metal salt precursor. The reaction liquid storage tank 7 is connected to the nanoparticle generator through the sampling pipeline, the nanoparticle generator is connected to the product cooler 2 through the corresponding delivery pipeline, the product cooler 2 is connected to the product collector 3 through the corresponding delivery pipeline, the sampling valve 8 and the sampling pump 9 are arranged on the sampling pipeline and are both connected to the controller. Under the control of the controller, the sampling valve 8 and the sampling pump 9 regulate the fluid flow rate and residence time in the reaction pipeline. The pipe diameter sizes of all the delivery pipelines range from 0.05 to 20 mm. The sampling valve 8 is a flow controller. The sampling pump 9 is a metering pump.
[0072] The nanoparticle generator is used to heat the reaction liquid flowing through it by means of magnetic vortex energy transfer, so that the reactants undergo a chemical reaction under the action of the magnetic vortex to generate inorganic nanoparticles. The nanoparticle generator includes a magnetic vortex reactor unit 4, a temperature feedback unit 5, and a pressure feedback unit 6. The magnetic vortex reactor unit 4 is composed of a section of reaction pipeline and a heater. The reaction pipeline is a millimeter fluid system, and the pipe diameter size of the reaction pipeline is 0.05 to 20 mm. One end of the reaction pipeline is communicated with the reaction liquid storage tank 7 through the sampling pipeline, the other end of the reaction pipeline is communicated with the product cooler 2, the heater realizes precise temperature control, and the temperature range of the reaction pipeline is 0 to 500 °C. In the nanoparticle generator, the heater generates a magnetic vortex for the reaction pipeline by controlling the magnetic field intensity of the alternating current coil, so that the reaction liquid flowing through the reaction pipeline is in a preset condition under the electromagnetic action, and thus a reaction occurs to generate inorganic nanoparticles.
[0073] The material of the reaction pipeline is a metal material, including one or more of carbon steel, Hastelloy, 304 stainless steel, 316 stainless steel, 316L stainless steel, chrome molybdenum alloy steel, low alloy high strength steel, pure copper, brass, Inconel alloy, pure titanium, titanium alloy, hot-dip galvanized steel, pure lead, duplex stainless steel, super stainless steel, etc., to ensure good electrical conductivity and heating efficiency during the continuous magnetic vortex flow process.
[0074] The temperature feedback unit 5 is connected to the controller. The temperature feedback unit 5 is responsible for detecting the temperature of the fluid in the reaction pipe and feeding back the temperature signal to the controller, so that the controller can control the reaction temperature in the reaction pipe according to the received temperature signal. The temperature feedback unit 5 can be a temperature sensor.
[0075] The pressure feedback unit 6 is connected to the controller. The pressure feedback unit 6 is responsible for detecting the pressure in the reaction pipe and feeding back the pressure signal to the controller, so that the controller can adjust the flow rate of the reaction liquid delivery system and the pressure corresponding to the reaction pipe according to the received pressure signal. The pressure feedback unit 6 can be a pressure sensor.
[0076] The controller is used to control and monitor the working states of the nanoparticle generator and the reaction liquid delivery system, ensuring that the reaction liquid in the nanoparticle generator reacts under preset conditions. By controlling the reaction temperature and reaction pressure, the reaction liquid in the reaction pipe can reach the preset conditions, thereby generating inorganic nanoparticles with more uniform sizes. The controller can be a computer, an industrial control computer or a microcontroller.
[0077] The product cooler 2 is used to cool the inorganic nanoparticles generated by the reaction. The product cooler can adopt an air cooling device or a liquid cooling device.
[0078] The product collector 3 is used to collect the inorganic nanoparticles obtained by cooling.
[0079] The back pressure valve 1 is arranged on the delivery pipe between the product cooler 2 and the product collector 3. It can be one or a combination of multiple valves, and is used to control the pressure of the reaction system to meet the pressure requirements of the reaction system.
[0080] Example 2 Hybrid heating continuous flow synthesis device:
[0081] See Figure 2As shown in the figure, the hybrid heating continuous flow synthesis device of this embodiment adopts a combination of reactors with two different heating methods, that is, an electric heating reactor, namely the spiral nanoparticle generator 11, is added on the basis of Embodiment 1. A spiral reaction pipeline is arranged in the spiral nanoparticle generator 11, and the spiral reaction pipeline is heated by direct current. The pipe diameter size of the spiral reaction pipeline is 0.05 - 20 mm. The inlet of the spiral reaction pipeline is connected to the outlet of the nanoparticle generator, and the outlet of the spiral reaction pipeline is connected to the inlet of the product cooler. Moreover, a temperature feedback unit 5 for detecting the temperature in the spiral reaction pipeline and a pressure feedback unit 6 for detecting the pressure in the spiral reaction pipeline are equipped in the spiral nanoparticle generator 11, and both the temperature feedback unit 5 and the pressure feedback unit 6 are connected to the controller. The nanoparticle generator has a faster heating-up time, while the spiral nanoparticle generator 11 has a longer reaction time. The combination of the two heating methods is suitable for the rapid nucleation and slow growth process of nanoparticles. The nanoparticle generator is connected to the spiral nanoparticle generator 11 through a pipeline to form a continuous flow reaction path.
[0082] The settings of the nanoparticle generator, the product cooler 2, the product collector 3, the reaction liquid delivery system, the back pressure valve 1 and the controller in this embodiment are the same as those in Embodiment 1.
[0083] Embodiment 3: Multi-combination magnetic vortex continuous flow synthesis device
[0084] See Figure 3 As shown in the figure, the nanoparticle generator of the multi-combination magnetic vortex continuous flow synthesis device of this embodiment includes multiple nanoparticle generator units, that is, on the basis of Embodiment 1, one nanoparticle generator unit is improved to multiple series-connected nanoparticle generator units 4, and a corresponding temperature feedback unit 5 and a corresponding pressure feedback unit 6 are equipped on each nanoparticle generator unit 4 to ensure that the temperature can change as required during the reaction. The reaction liquid is transported into the nanoparticle generator through the sampling valve 8 and the sampling pump 9, and undergoes a heating reaction through multiple series-connected nanoparticle generator units 4.
[0085] Each of the nanoparticle generator units 4 adopts a modular design. Adjacent two sections of the reaction pipes are connected through corresponding connecting pipes to form a continuously flowing reaction path. The set temperatures of each of the nanoparticle generator units 4 can be the same to ensure uniform heating throughout the synthesis process; or they can be different to achieve the separation of the nucleation and growth processes during the nanoparticle synthesis process and meet the requirements of different synthesis temperatures. The heating method of the nanoparticle generator unit 4 can also be replaced with electric heating, aluminum block heating, or oil bath heating. For electromagnetic heating, the reaction pipe length of each of the nanoparticle generator units 4 is adjustable to control the heating time.
[0086] The product cooler 2, product collector 3, reaction liquid delivery system, back pressure valve 1, and controller in this embodiment are arranged in the same way as in Embodiment 1.
[0087] Embodiment 4: Multi-injection channel magnetic vortex continuous flow synthesis device:
[0088] See Figure 4 As shown, the reaction liquid delivery system in the multi-injection channel magnetic vortex continuous flow synthesis device of this embodiment includes at least two reaction liquid storage tanks 7, at least two injection pipes, multiple delivery pipes, a reagent mixer 10, at least two injection valves 8, and at least two injection pumps 9.
[0089] Each of the reaction liquid storage tanks 7 is respectively used to independently store the reagent raw materials required for preparing the reaction liquid containing the metal salt precursor. The reagent mixer 10 is used to mix the reagent raw materials delivered from each of the reaction liquid storage tanks 7, thereby preparing the reaction liquid containing the metal salt precursor, and then introducing it into the nanoparticle generator for reaction.
[0090] The reagent mixer 10 is a T-shaped, Y-shaped, or static mixer. Each inlet end of the reagent mixer 10 is connected to each of the reaction liquid storage tanks 7 through the corresponding injection pipes respectively. The outlet end of the reagent mixer 10 is connected to the nanoparticle generator through a delivery pipe. The nanoparticle generator is connected to the product cooler 2 through a delivery pipe. The product cooler 2 is connected to the product collector 3 through a delivery pipe. The pipe diameters of the injection pipes and the delivery pipes range between 0.05 and 20 mm.
[0091] A set of corresponding injection valves 8 and injection pumps 9 are arranged on each of the injection pipes, and each set of injection valves 9 and injection pumps 9 are connected to the controller. Under the control of the controller, each set of injection valves 8 and injection pumps 9 regulate the fluid flow rate and residence time in the reaction pipe where they are located.
[0092] The settings of the product nanoparticle generator, cooler 2, product collector 3, back pressure valve 1, and controller in this embodiment are the same as those in Embodiment 1.
[0093] Method for continuously preparing inorganic nanoparticles by magnetic vortex flow in Embodiment 5:
[0094] The preparation method of this embodiment is realized based on the magnetic vortex continuous flow synthesis device in any one of Embodiments 1-3, and specifically includes the following steps:
[0095] Step 1) Dissolve the organometallic compound or metal salt compound precursor and the small molecule with an alkyl chain together in a solvent to prepare a reaction solution, and inject it into the reaction solution storage tank 7.
[0096] The concentration of the organometallic compound or the inorganic metal salt compound is 0.001-1 mol / L, and the preferred concentration is 0.01-0.1 mol / L.
[0097] The organometallic compound is an organometallic complex containing a transition metal or a rare earth metal, specifically an organometallic complex of iron, cobalt, nickel, manganese or lanthanide rare earth metal, and its ligands include acetylacetone, carbonyl, phenylacetylacetone, and cyclopentadiene. Preferred embodiments of the organometallic compound include, but are not limited to: iron(III) acetylacetonate, iron(II) acetylacetonate, iron pentacarbonyl, iron(III) phenylacetylacetonate, manganese(II) acetylacetonate, manganese(III) phenylacetylacetonate, nickel(II) acetylacetonate, nickel tetracarbonyl, cobalt(II) acetylacetonate, dicobalt octacarbonyl, gadolinium(III) acetylacetonate, gadolinium(III) tricyclopentadienyl, dysprosium(III) acetylacetonate, holmium(III) acetylacetonate, etc., or a mixture of one or more of them.
[0098] The metal salt compound is a salt containing a transition metal and a rare earth metal or its hydrate, specifically an oleate, stearate, fatty acid salt, trifluoroacetate, gluconate, citrate, oxalate, chloride, sulfate, nitrate of iron, cobalt, nickel, manganese or lanthanide rare earth metal and its hydrate. Specific examples of the metal salt compound include, but are not limited to: iron oleate, iron stearate, iron acetate, iron citrate, iron oxalate, ferric chloride, ferrous chloride, ferric chloride tetrahydrate, ferric chloride hexahydrate, iron nitrate, iron sulfate, cobalt oleate, cobalt stearate, cobalt acetate, cobalt citrate, cobalt oxalate, cobalt decanoate, cobalt chloride, manganese acetate, manganese oxalate, manganese chloride, manganese nitrate, manganese sulfate, gadolinium oleate, gadolinium stearate, gadolinium acetate, gadolinium chloride, gadolinium chloride trihydrate, gadolinium chloride hexahydrate, gadolinium nitrate, dysprosium acetate, dysprosium chloride, dysprosium chloride trihydrate, dysprosium chloride hexahydrate, dysprosium nitrate, holmium acetate, holmium chloride, holmium chloride trihydrate, holmium chloride hexahydrate, holmium nitrate, erbium acetate, erbium chloride, erbium chloride trihydrate, erbium chloride hexahydrate, erbium nitrate, thulium acetate, thulium chloride, thulium chloride trihydrate, thulium chloride hexahydrate, thulium nitrate, etc.
[0099] The concentration of the small molecule with an alkyl chain is 0.001 - 10 mol / L, preferably 0.01 - 0.6 mol / L.
[0100] The small molecule with an alkyl chain is a small molecule amine, small molecule carboxylic acid, small molecule alcohol, or small molecule phosphine with an alkyl chain.
[0101] The solvent is one or a mixture of several of phenyl ether, anisole, dibenzyl ether, 1 - octadecene, oleic acid, oleylamine, trioctylamine, methanol, ethanol, isopropanol, n - butanol, cyclohexane, water, or 2 - pyrrolidone, or derivatives and analogs of the above solvents.
[0102] In step 2), under the control of the controller, the injection valve 8 and the injection pump 9 deliver the reaction solution from the reaction solution reservoir 7 into the nanoparticle generator at a certain flow rate and for a certain time.
[0103] In the nanoparticle generator, the size range of all pipelines is 0.05 - 20 mm. The flow rate of the reaction solution is controlled at 0.02 - 1000 mL / min, preferably 0.1 - 500 mL / min. The reaction temperature is controlled between 120 - 500 °C, preferably 180 - 300 °C. The reaction pressure is controlled at 1 - 300 atmospheres, preferably 3 - 100 atmospheres. The residence time of the reaction solution in the reaction pipeline is controlled at 0.01 - 60 min.
[0104] In the nanoparticle generator, the heater performs magnetic vortexing on the reaction pipeline by controlling the magnetic field intensity of the alternating current coil, so that the reaction solution flowing through the reaction pipeline is under preset conditions under electromagnetic action, and thus reacts to generate inorganic nanoparticles.
[0105] During the magnetic vortexing process, the temperature feedback unit 5 and the pressure feedback unit 6 respectively monitor the reaction temperature and reaction pressure in the reaction pipeline, and feed the temperature signal and pressure signal back to the controller, so that the controller can respectively adjust the heating temperature of the alternating current coil and the flow rate of the injection valve 8 according to the monitored temperature signal and pressure signal, ensuring that the reaction solution is always under preset conditions in the reaction pipeline.
[0106] During the application process, by changing the reaction conditions, including the concentration of the metal precursor, the concentration of the small molecule with an alkyl chain, the reaction temperature, the reaction pressure, the residence time, the flow rate of the reaction solution, the size of the reactor channel, etc., inorganic nanoparticles with different sizes and particle size distributions can be prepared.
[0107] In step 3), driven by the flow rate of the next wave of reaction solution, the generated inorganic nanoparticles enter the product cooler 2 with the fluid for cooling to prevent particle agglomeration.
[0108] In step 4), driven by the flow rate of the next wave of reaction solution, the cooled inorganic nanoparticles enter the product collector 3 with the fluid.
[0109] Example 6 Method for Preparing Inorganic Nanoparticles by Magnetic Vortex Continuous Flow with Multiple Sampling Channels:
[0110] The preparation method of this example is realized based on the multiple sampling channel magnetic vortex continuous flow synthesis device of Example 4, and specifically includes the following steps:
[0111] Step 1) Dissolve the precursor of the organometallic compound or inorganic metal salt compound in a solvent to obtain a precursor solution, and inject it into the corresponding reaction solution reservoir.
[0112] The concentration of the precursor solution is 0.001 - 1 mol / L, and the preferred concentration is 0.01 - 0.1 mol / L.
[0113] The organometallic compound is an organic complex containing a transition metal or a rare earth metal, specifically an iron, cobalt, nickel, manganese or lanthanide rare earth metal organic complex, and its ligands include acetylacetone, carbonyl, phenylacetylacetone, cyclopentadiene. Preferred examples of the organometallic compound include, but are not limited to: iron(III) acetylacetonate, iron(II) acetylacetonate, iron pentacarbonyl, iron(III) phenylacetylacetonate, manganese(II) acetylacetonate, manganese(III) phenylacetylacetonate, nickel(II) acetylacetonate, nickel tetracarbonyl, cobalt(II) acetylacetonate, dicobalt octacarbonyl, gadolinium(III) acetylacetonate, gadolinium(III) tricyclopentadienyl, dysprosium(III) acetylacetonate, holmium(III) acetylacetonate, etc., or a mixture of one or more of them.
[0114] The metal salt compound is a salt containing a transition metal and a rare earth metal or its hydrate, specifically an oleate, stearate, fatty acid salt, trifluoroacetate, gluconate, citrate, oxalate, chloride, sulfate, nitrate of iron, cobalt, nickel, manganese or lanthanide rare earth metal and its hydrate. Specific examples of the metal salt compound include, but are not limited to: iron oleate, iron stearate, iron acetate, iron citrate, iron oxalate, ferric chloride, ferrous chloride, ferric chloride tetrahydrate, ferric chloride hexahydrate, iron nitrate, iron sulfate, cobalt oleate, cobalt stearate, cobalt acetate, cobalt citrate, cobalt oxalate, cobalt decanoate, cobalt chloride, manganese acetate, manganese oxalate, manganese chloride, manganese nitrate, manganese sulfate, gadolinium oleate, gadolinium stearate, gadolinium acetate, gadolinium chloride, gadolinium chloride trihydrate, gadolinium chloride hexahydrate, gadolinium nitrate, dysprosium acetate, dysprosium chloride, dysprosium chloride trihydrate, dysprosium chloride hexahydrate, dysprosium nitrate, holmium acetate, holmium chloride, holmium chloride trihydrate, holmium chloride hexahydrate, holmium nitrate, erbium acetate, erbium chloride, erbium chloride trihydrate, erbium chloride hexahydrate, erbium nitrate, thulium acetate, thulium chloride, thulium chloride trihydrate, thulium chloride hexahydrate, thulium nitrate, etc.
[0115] Step 2) Select a small molecule with an alkyl chain as a stabilizer and inject it into the corresponding reaction solution reservoir.
[0116] The concentration of the stabilizer is 0.001 - 10 mol / L, preferably 0.01 - 0.6 mol / L.
[0117] The small molecule with an alkyl chain is a small molecule amine, a small molecule carboxylic acid, a small molecule alcohol, and a small molecule phosphine with an alkyl chain.
[0118] Step 3) Select one or a mixture of phenyl ether, anisole, dibenzyl ether, 1-octadecene, oleic acid, oleylamine, trioctylamine, methanol, ethanol, isopropanol, n-butanol, cyclohexane, water, or 2-pyrrolidone, or derivatives and analogs of the above solvents as the solvent, and inject it into the corresponding reaction solution reservoir.
[0119] Step 4) The deoxygenated precursor solution, the small molecule with an alkyl chain, and the solvent are respectively incorporated into the reagent mixer 10 through their respective corresponding injection pipes, injection valves 8, and injection pumps 9 for mixing to prepare a reaction solution.
[0120] Step 5) Then, under the action of the corresponding injection valve 8 and injection pump 9, the reaction solution is transported from the reagent mixer 10 to the nanoparticle generator at a certain flow rate and for a certain time. In the case of multiple injection channels, the concentration and ratio of each reactant can be controlled by regulating the flow rate of the reaction solution in each injection channel, thereby preparing different inorganic nanoparticles.
[0121] In the nanoparticle generator, the size range of all pipes is 0.05 - 20 mm. The flow rate of the reaction solution in each injection pipe is controlled at 0.02 - 1000 mL / min, preferably 0.1 - 500 mL / min; the reaction temperature is controlled between 120 - 500 °C, preferably 180 - 300 °C. The reaction pressure is controlled at 1 - 300 atmospheres, preferably 3 - 100 atmospheres. The residence time of the reaction solution in the reaction pipe is controlled at 0.01 - 60 min.
[0122] In the nanoparticle generator, under the regulation of the controller, the heater electromagnetically heats the reaction pipe by controlling the magnetic field intensity of the alternating current coil, so that the reaction solution flowing through the reaction pipe is in a preset condition under the electromagnetic action, thereby reacting to generate inorganic nanoparticles.
[0123] During the electromagnetic heating process, the temperature feedback unit 6 and the pressure feedback unit 7 respectively monitor the reaction temperature and reaction pressure in the reaction pipe, and feed the temperature signal and pressure signal back to the controller, so that the controller can respectively regulate the heating temperature of the alternating current coil and the flow rate of the injection valve 8 according to the monitored temperature signal and pressure signal to ensure that the reaction solution is always in a preset condition in the reaction pipe.
[0124] During the application process, by changing the reaction conditions, including the concentration of metal precursors, the concentration of small molecules with alkyl chains, reaction temperature, reaction pressure, residence time, reaction solution flow rate, reactor channel size, etc., inorganic nanoparticles with different sizes and particle size distributions can be prepared.
[0125] Step 3) Driven by the flow rate of the next wave of reaction solution, the inorganic nanoparticles generated by the reaction enter the product cooler 2 with the fluid for cooling to prevent particle agglomeration.
[0126] Step 4) Driven by the flow rate of the next wave of reaction solution, the cooled inorganic nanoparticles enter the product collector 3 with the fluid.
[0127] Example 7 Inorganic Nanoparticles:
[0128] The inorganic nanoparticles of this example are prepared by the preparation method of Example 5 or 6, with a particle size of 1 - 100 nanometers, and are oxides of iron, cobalt, nickel, manganese, or iron\cobalt\nickel\gadolinium\terbium\dysprosium\holmium\erbium\thulium.
[0129] The surface of the inorganic nanoparticles of this example is modified with one or more of small molecule amines, small molecule carboxylic acids, small molecule alcohols, and small molecule phosphines with alkyl chains, and the number of CH 2 units in the alkyl chain is 4 - 24, preferably 12 - 18, such as oleylamine, dodecylamine, myristic acid, oleic acid, 1,2-dodecanediol, octadecanol, etc.
[0130] Example 7 - 1
[0131] The inorganic nanoparticles of this example are prepared by using the magnetic vortex continuous flow synthesis device of Example 1 and the method for continuously preparing inorganic nanoparticles by magnetic vortex of Example 5. The specific steps are as follows:
[0132] Dissolve 7.0 g of iron acetylacetonate, 36.0 g of oleic acid, and 35.5 g of oleylamine in 1 L of toluene. Pump the obtained reaction solution into the magnetic vortex continuous flow synthesis device of Example 1. Heat the reactor to be a nanoparticle generator, with the length of the alternating current coil being 20 cm and the inner diameter of the reaction pipe being 8.0 mm. Control the reaction temperature in the reactor to be 300 °C, the residence time to be 2 s, the reaction flow rate to be 15 mL / min, and the reaction pressure to be 50 atmospheres.
[0133] After the reaction solution is cooled to room temperature by the cooler, it enters the sample collector.
[0134] Dissolve the obtained nanoparticles in cyclohexane, and use a transmission electron microscope (TEM) to characterize the obtained inorganic nanoparticles. See Figure 5 as shown, Figure 5Transmission electron microscopy (TEM) image (A) and histogram of particle size distribution (B) of the inorganic nanoparticles obtained in this example. It can be seen from the TEM image that the nanoparticles are approximately spherical, with an average particle size of 3.9 nm and a relative standard deviation of 10.3% in size, indicating good uniformity. After modification with bisphosphonate polyethylene glycol, the nanoparticles are water-soluble, with an r1 relaxation rate of 4.36 mM -1 ·s -1 , an r2 relaxation rate of 15.60 mM -1 ·s -1 , and an r2 / r1 ratio of 3.6, showing excellent T1 magnetic resonance imaging performance.
[0135] Example 7-2
[0136] The inorganic nanoparticles in this example were prepared using the hybrid magnetic vortex continuous flow synthesis device of Example 2 and the method for preparing inorganic nanoparticles by magnetic vortex continuous flow of Example 5. The specific steps are as follows:
[0137] 7.0 g of iron acetylacetonate, 36.0 g of oleic acid, and 35.5 g of oleylamine were dissolved in 1 L of toluene. The resulting reaction solution was pumped into the hybrid magnetic vortex continuous flow synthesis device, and the reactor used a multi-combination heating reactor. In the first-stage nanoparticle generator, the length of the alternating current coil was 20 cm, the inner diameter of the reaction pipe was 8.0 mm, the reaction temperature in the reactor was controlled at 240 °C, and the residence time was 2 s. In the second-stage tubular reactor, the inner diameter was 3.0 mm, the reaction temperature in the reactor was controlled at 40 °C, the residence time was 4 min, the reaction flow rate was 15 mL / min, and the reaction pressure was 50 atmospheres.
[0138] After the reaction solution was cooled to room temperature by a cooler, it entered the sample collector.
[0139] The obtained nanoparticles were dissolved in cyclohexane, and the resulting inorganic nanoparticles were characterized using transmission electron microscopy (TEM). See Figure 6 shown Figure 6 for the TEM image (A) and histogram of particle size distribution (B) of the obtained inorganic nanoparticles. It can be seen from the TEM image that the nanoparticles are approximately spherical, with an average particle size of 10.2 nm and a relative standard deviation of 16.7% in size, indicating good uniformity. See Figure 7 shown Figure 7 for the hysteresis loop of the obtained Fe 3 O 4 inorganic nanoparticles at 298 K. Its saturation magnetization is 46.2 emu / g, indicating that the prepared nanoparticles have strong magnetism and superparamagnetism at room temperature.
[0140] In summary, the present invention proposes a continuous flow synthesis device based on magnetic vortices, which realizes the efficient, stable, and controllable synthesis of inorganic nanoparticles by combining the advantages of magnetic vortex heating technology and continuous flow synthesis technology. This device can not only significantly improve the yield and product quality, but also has good scalability and is suitable for industrial production.
[0141] Continuous flow synthesis technology is a method for continuously synthesizing chemical substances by carrying out reactions in a continuous flow reactor. Compared with the traditional batch reaction method, continuous flow synthesis technology has the following advantages: 1. High-efficiency production: The continuous flow reactor can achieve continuous feeding of reactants and continuous discharging of products, greatly improving production efficiency. 2. Precise control of reaction conditions: By adjusting parameters such as flow rate, reaction time, and temperature, the reaction conditions can be precisely controlled to ensure the quality and consistency of the products. 3. Easy to scale up: The design of the continuous flow reactor makes it easy to scale up and is suitable for large-scale industrial production.
[0142] Specifically, the present invention realizes the real-time adjustment of the reaction temperature and flow rate by precisely controlling the reaction conditions, ensuring the stability of the reaction process and the uniformity of the generated particles. In short, based on solving the problems of the existing technology, the present invention provides an innovative device and method for synthesizing inorganic nanoparticles, which has broad application prospects and significant technical advantages.
[0143] The above are only the preferred embodiments of the present invention and are not intended to limit the present invention. For those skilled in the art, the present invention can have various changes and modifications. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.
Claims
1. A device for synthesizing inorganic nanoparticles by continuous flow through magnetic vortex energy transfer, characterized in that: The invention at least comprises a nanoparticle generator, a reaction liquid delivery system, a back pressure valve (1), a controller, a product cooler (2) and a product collector (3); wherein: The reaction liquid delivery system is used to deliver the reaction liquid containing the metal salt precursor to the nanoparticle generator at a certain flow rate for reaction, and then deliver the inorganic nanoparticles generated by the reaction to the product collector (3) through the product cooler (2) at a certain flow rate; The nanoparticle generator is used to heat the reaction liquid flowing therethrough by means of magnetic vortex energy transfer, so that the reactants undergo a chemical reaction under the action of the magnetic vortex to generate inorganic nanoparticles; The back pressure valve (1) is connected between the product cooler (2) and the product collector (3) and is used to control the pressure required by the reaction system; The controller is used to monitor the working status of the nanoparticle generator and the reaction liquid delivery system to ensure that the reaction liquid in the nanoparticle generator reacts under preset conditions; The product cooler (2) is used to cool the inorganic nanoparticles generated by the reaction; The product collector (3) is used to collect the cooled inorganic nanoparticles.
2. The device for synthesizing inorganic nanoparticles by continuous flow through magnetic vortex energy transfer according to claim 1, characterized in that: The nanoparticle generator comprises at least one magnetic vortex reactor unit (4), at least one temperature feedback unit (5) and at least one pressure feedback unit (6); The magnetic vortex reactor unit (4) is composed of a reaction pipe and a heater; the reaction pipe is a millimeter fluid system, and the diameter of the reaction pipe is 0.05-20 mm; one end of the reaction pipe is connected to the reaction liquid delivery system, and the other end of the reaction pipe is connected to the product cooler (2); the heater is connected to the controller signal to achieve accurate control of the heating temperature; the heater controls the magnetic field strength of the alternating current coil to perform a magnetic vortex on the reaction pipe, so that the reaction liquid flowing through the reaction pipe is in a preset condition under the electromagnetic effect, thereby reacting to generate inorganic nanoparticles; When the nanoparticle generator comprises a plurality of nanoparticle generator units (4) connected in series, each of the nanoparticle generator units (4) adopts a modular design, and two adjacent sections of the reaction pipeline are connected via corresponding connecting pipelines; The temperature feedback unit (5) is connected to the controller, and each of the temperature feedback units (5) is responsible for detecting the temperature in the corresponding reaction pipe and feeding back the temperature signal to the controller, so that the controller adjusts the temperature of the reaction liquid in the corresponding reaction pipe according to the received temperature signal; The pressure feedback unit (6) is connected to the controller, and each of the pressure feedback units (6) is responsible for detecting the pressure in the corresponding reaction pipeline and feeding back the pressure signal to the controller, so that the controller can adjust the flow rate of the reaction liquid and the reaction pressure in the corresponding reaction pipeline according to the received pressure signal; By precisely controlling the reaction temperature and reaction pressure in the nanoparticle generator, flow synthesis of inorganic nanoparticles with more uniform sizes can be achieved.
3. The device for synthesizing inorganic nanoparticles by continuous flow through magnetic vortex energy transfer according to claim 2, characterized in that: The temperature of the reaction pipe under the control of the heater ranges from 0 to 500°C.
4. The device for synthesizing inorganic nanoparticles by continuous flow through magnetic vortex energy transfer according to claim 2, characterized in that: The material of the reaction pipe is a metal material, including one or more of carbon steel, Hastelloy, 304 stainless steel, 316 stainless steel, 316L stainless steel, chromium-molybdenum alloy steel, low alloy high strength steel, pure copper, brass, Inconel alloy, pure titanium, titanium alloy, hot-dip galvanized steel, pure lead, duplex stainless steel, and super stainless steel.
5. The device for synthesizing inorganic nanoparticles by continuous flow through magnetic vortex energy transfer according to claim 1, characterized in that: The reaction liquid delivery system comprises a reaction liquid storage container (7), a sample injection pipeline, a plurality of delivery pipelines, a sample injection valve (8) and a sample injection pump (9); The reaction liquid storage device is used to store the prepared reaction liquid containing the metal salt precursor; the reaction liquid storage device (7) is connected to the nanoparticle generator via the injection pipeline, the nanoparticle generator is connected to the product cooler (2) via the corresponding delivery pipeline, the product cooler (2) is connected to the product collector (3) via the corresponding delivery pipeline, the injection valve (8) and the injection pump (9) are arranged on the injection pipeline and are both connected to the controller. Under the control of the controller, the injection valve (8) and the injection pump (9) regulate the fluid flow rate and residence time in the reaction pipeline; the diameter of the delivery pipeline ranges from 0.05 to 20 mm.
6. The device for synthesizing inorganic nanoparticles by continuous flow through magnetic vortex energy transfer according to claim 1, characterized in that: The reaction liquid delivery system comprises a plurality of reaction liquid storages (7), a plurality of injection pipes, a plurality of delivery pipes, at least one reagent mixer (10), a plurality of injection valves (8) and a plurality of injection pumps (9); Each of the reaction liquid storage devices (7) is used to independently store reagent raw materials required for preparing a reaction liquid containing a metal salt precursor; the reagent mixer (10) is used to mix the reagent raw materials delivered by each of the reaction liquid storage devices (7) to prepare a reaction liquid containing a metal salt precursor; the reagent mixer (10) is connected to each of the reaction liquid storage devices (7) via a corresponding sample introduction pipeline, the reagent mixer (10) is connected to the nanoparticle generator via a corresponding delivery pipeline, and the nanoparticle generator is connected to the product cooler via a corresponding delivery pipeline. The product cooler and the product collector are connected by corresponding delivery pipelines; each of the injection pipelines is provided with a corresponding group of the injection valves (8) and the injection pumps (9), and each group of the injection valves (8) and the injection pumps (9) is connected to the controller. Under the control of the controller, each group of the injection valves (8) and the injection pumps (9) regulates the flow rate and residence time of the fluid in the reaction pipeline where they are located; the diameter of the injection pipeline and the delivery pipeline ranges from 0.05 to 20 mm.
7. The device for synthesizing inorganic nanoparticles by continuous flow through magnetic vortex energy transfer according to claim 6, characterized in that: The reagent mixer (10) is a T-type, Y-type or static mixer.
8. A method for synthesizing inorganic nanoparticles by continuous flow through magnetic vortex energy transfer, characterized in that: The method is implemented by using a device for continuously synthesizing inorganic nanoparticles by magnetic vortex energy transfer as described in any one of claims 1 to 7, comprising the following steps: Step 1) The injection valve and the injection pump, under the control of the controller, transport the prepared reaction liquid from the reaction liquid storage (7) into the nanoparticle generator; in the nanoparticle generator, the heater makes the reaction liquid flowing through the reaction pipe in a high temperature state under the action of the magnetic vortex, thereby generating inorganic nanoparticles; Step 2) driven by the sample injection pump, the inorganic nanoparticles generated by the reaction enter the product cooler (2) along with the fluid for cooling; Step 3) Driven by the injection pump, the cooled inorganic nanoparticles enter the product collector (10) along with the fluid.
9. The method for synthesizing inorganic nanoparticles by continuous flow through magnetic vortex energy transfer according to claim 8, characterized in that: In step 1, The flow rate of the reaction solution is controlled at 0.02-1000 mL / min; The reaction temperature is controlled at 120-500°C; The reaction pressure is controlled at 1 to 300 atmospheres; The residence time of the reaction liquid in the reaction pipe is controlled at 0.01 to 60 minutes.
10. The method for synthesizing inorganic nanoparticles by continuous flow through magnetic vortex energy transfer according to claim 8, characterized in that: In step 1, During the heating process, the temperature feedback unit and the pressure feedback unit monitor the reaction temperature and the reaction pressure in the reaction pipeline respectively, and adjust the heating temperature of the reaction pipeline and the pressure of the back pressure valve (1) according to the temperature signal and the pressure signal, so as to ensure that the reaction liquid is always in the preset condition in the reaction pipeline.