Flow-type preparation method and device for NANO material

Abstract

A flow-type continuous preparation method for a nano material, comprising: step S1, putting a metal ion solution and a micro-nano-scale metal solution into a reactant container; step S2, separately controlling the metal ion solution and the micro-nano-scale metal solution to simultaneously flow into a reaction channel at a specific flow rate, such that the two solutions are in full contact with each other and undergo a displacement reaction to form a mixed reaction solution, the mixed reaction solution comprising a complete reaction solution and an incomplete reaction solution; step S3, controlling the complete reaction solution and the incomplete reaction solution to respectively flow into a particle collector and a solution collector; step S4, extracting the incomplete reaction solution from the solution collector by means of a return pipe to allow same to flow back into the reactant container; and step S5, repeating steps S1 to S4. The present invention further relates to a device for implementing the flow-type continuous preparation method for a nano material, achieves continuous production, greatly increases the utilization rate of reaction solutions, reduces cost, is suitable for the industrial field, and has great prospects in industrialization.

Description

A flow-type preparation method and device for nanomaterials

[0001] CROSS-REFERENCE TO RELATED APPLICATIONS

[0002] This application claims priority to the Chinese patent application with application number 202311488007.8 filed with the Chinese Patent Office on November 8, 2023, entitled "A Flow-type Preparation Method and Device for Nanomaterials", the entire contents of which are incorporated by reference into this application. Technical Field

[0003] The present invention relates to the field of nanomaterial preparation technology, and in particular to a flow-type preparation method and device for nanomaterials. Background Art

[0004] The nanostructure of micro- and nanomaterials is a novel system constructed or constructed according to specific rules based on nanoscale material units. These include nanoarray systems, mesoporous assembly systems, and thin-film mosaic systems. This results in nanoparticles exhibiting thermal, magnetic, optical, sensitive, and surface stability properties that differ from those of normal particles, leading to their widespread application. Micro- and nanomaterials generally refer to materials with sizes in the micrometer and nanometer range, exhibiting unique physical, chemical, and biological properties. Micro- and nanomaterials can be single crystals, polycrystalline, or amorphous. Common micro- and nanomaterials include nanoparticles, nanowires, nanosheets, and nanotubes. Their size not only influences their electronic, optical, and thermal properties, but also their oxidation and reduction reactions. For example, the core-shell structure of a core-shell material is an ordered assembly formed by encapsulating one micro- and nanomaterial with another through chemical bonds or other interactions. Encapsulation techniques can tailor the surface properties of the core particles, modifying their surface charge, functional groups, and reactivity, while improving their stability and dispersibility. Their unique structural characteristics can impart diverse properties to the material, playing an important role in catalysis, photocatalysis, batteries, and gas storage and separation.

[0005] However, existing methods for preparing metal nanoparticles, including chemical reduction, vapor deposition, hydrothermal synthesis, sol-gel, photochemical, microemulsion, template, phase transfer, ultrasound, and radiation, are often susceptible to reaction conditions, making precise control difficult. Furthermore, their morphology is often limited by the raw material container or the template used during synthesis, making continuous and large-scale production difficult. These issues hinder the mass production of nanomaterials.

[0006] Therefore, there is an urgent need to provide a flow-type preparation method and device for nanomaterials to solve the above problems.

[0007] Summary of the Invention

[0008] In view of the shortcomings of the related art, the present invention proposes a flow-type preparation method and device for nanomaterials.

[0009] In order to solve the above technical problems, an embodiment of the present invention provides a continuous preparation method of nanomaterials, which includes:

[0010] Step S1, placing one or more metal ion solutions and micro-nano metal solutions in a reactant container;

[0011] Step S2, controlling the metal ion solution and the micro-nano metal solution to flow simultaneously into the reaction channel at specific flow rates, so that the metal ion solution and the micro-nano metal solution are in full contact and undergo a displacement reaction to form a reaction mixture solution, wherein the reaction mixture solution includes a completely reacted solution and an unreacted completely solution;

[0012] Step S3, controlling the completely reacted solution and the unreacted completely reacted solution to flow into a particle collector and a solution collector respectively;

[0013] Step S4, drawing the unreacted complete solution from the solution collector through a reflux pipe and returning it to the reactant container;

[0014] Step S5, looping the process from step S1 to step S4.

[0015] Preferably, the micro-nano metal solution comprises micro-nano metal particles and a solvent.

[0016] Preferably, the micro-nano metal particles are bidirectional metal particles.

[0017] Preferably, the solvent includes deionized water and an organic solvent, and the organic solvent is an alcohol organic solvent or a ketone organic solvent.

[0018] Preferably, the flow rate of the metal ion solution and the micro-nano metal solution flowing into the reaction channel is 4:1 or 1:1 or 2:1.

[0019] Preferably, the reaction channel is controlled by applying any one of ultrasound, ultraviolet light and high temperature to the metal ion solution and the micro-nano metal solution, so that the metal ion solution and the micro-nano metal solution are fully contacted and a displacement reaction occurs to form a reaction mixed solution.

[0020] An embodiment of the present invention also provides a continuous preparation device for nanomaterials, including a reactant container, a particle collector arranged relative to the reactant container, a reaction channel connected to both the reactant container and the particle collector, a solution collector connected to the particle collector, and a reflux mechanism connected to both the solution collector and the reactant container.

[0021] Preferably, the reactant container includes a first reaction container, a first supplementary channel and a first reflux port arranged on two opposite sides of the first reaction container, a second reaction container spaced apart from the first reaction container, a second supplementary channel and a second reflux port arranged on two opposite sides of the second reaction container, and a connecting pipe connected to the bottom of both the first reaction container and the second reaction container.

[0022] Preferably, the reaction channel includes a water bath ultrasonic container located between the connecting pipe and the particle collector and a hollow pipe located in the water bath ultrasonic container, one end of the hollow pipe is connected to the connecting pipe, and the other end of the hollow pipe is connected to the particle collector; the shape of the hollow pipe is linear or spiral.

[0023] Preferably, the particle collector includes a processing mechanism connected to one end of the hollow pipe away from the connecting pipe and a particle collecting mechanism that is detachably connected to the processing mechanism, the solution collector is connected to the particle collecting mechanism, and the reflux mechanism is simultaneously connected to the solution collector, the first reflux port and the second reflux port; the processing mechanism is a filter and / or a centrifuge.

[0024] Compared with the related art, the present invention provides a flow-type preparation method and device for nanomaterials. Under the setting of the communicating vessel principle, the metal ion solution and the micro-nano-scale metal solution undergo a replacement reaction in the reaction channel to form a reaction mixture solution. The reaction mixture solution includes a completely reacted solution and an unreacted solution. The reaction mixture solution then flows into a particle collector. The completely reacted solution forms the required nanomaterial particles, which will be adsorbed in the particle collector. The unreacted solution flows into the solution collector, and a reflux mechanism extracts the unreacted solution in the solution collector and refluxes the micro-nano-scale metal solution and the metal ion solution in the unreacted solution into corresponding reactant containers. The nanomaterial particles in the particle collector are then collected. The flow-type preparation method and device for nanomaterials provided by the present invention achieve large-scale flow-type continuous production of nanomaterial particles. At the same time, the completely reacted particles can be directly collected, effectively improving production efficiency and output. The method is particularly suitable for the industrial field and has good industrialization prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] The present invention will be described in detail below with reference to the accompanying drawings. The above and other aspects of the present invention will become clearer and easier to understand through the detailed description made with reference to the following drawings. In the accompanying drawings:

[0026] FIG1 is a schematic flow diagram of a flow-type preparation method of a nanomaterial according to the present invention;

[0027] FIG2 is a schematic structural diagram of a flow-type preparation device for nanomaterials according to the present invention;

[0028] FIG3 is a schematic structural diagram of another embodiment of a flow-type nanomaterial preparation device according to the present invention. DETAILED DESCRIPTION

[0029] The specific embodiments and examples described herein are specific embodiments of the present invention and are intended to illustrate the concepts of the present invention. They are illustrative and exemplary only and should not be construed as limiting the embodiments and scope of the present invention. In addition to the examples described herein, those skilled in the art may also employ other obvious technical solutions based on the claims and disclosure of this application. Such solutions, including any obvious substitutions and modifications of the embodiments described herein, are within the scope of protection of the present invention.

[0030] Referring to FIG1 , the present invention provides a flow-type preparation method for nanomaterials, comprising:

[0031] Step S1, placing one or more metal ion solutions and micro-nano metal solutions in a reactant container;

[0032] Step S2, controlling the metal ion solution and the micro-nano metal solution to flow simultaneously into the reaction channel at specific flow rates, so that the metal ion solution and the micro-nano metal solution are in full contact and undergo a displacement reaction to form a reaction mixture solution, wherein the reaction mixture solution includes a completely reacted solution and an unreacted completely solution;

[0033] Step S3, controlling the completely reacted solution and the unreacted completely reacted solution to flow into a particle collector and a solution collector respectively;

[0034] Step S4, drawing the unreacted complete solution from the solution collector through a reflux pipe and returning it to the reactant container;

[0035] Step S5, looping the process from step S1 to step S4.

[0036] In this embodiment, the micro-nano metal solution includes micro-nano metal particles and a solvent. The micro-nano metal particles are bimetallic particles, such as one or more of copper particles, antimony particles, zinc particles, and nickel particles. The solvent includes deionized water and an organic solvent, and the organic solvent is an alcohol or ketone.

[0037] Specifically, the flow rate of the metal ion solution and the micro-nanoscale metal solution into the reaction channel is 4:1, 1:1, or 2:1. The specific flow rate ratio is set according to different reaction solutions. For example, the reactant containers are used to hold a pretreated solution containing copper salts and a reduction system composed of the reducing agent ascorbic acid and the protective agent polyvinylpyrrolidone K30. Through the principle of communicating vessels, the flow rate ratio can generally be selected to be 1:1 or 2:1, depending on the specific experimental requirements and reaction conditions. If the reactant containers are used to hold the silver ammonia solution and the nano-copper particle containing ethanol solution, the flow rate on both sides can be controlled to 4:1 through the principle of communicating vessels.

[0038] In this embodiment, the reaction channel is controlled by applying any one of ultrasound, ultraviolet light and high temperature to the metal ion solution and the micro-nano metal solution, so that the metal ion solution and the micro-nano metal solution can fully contact each other to undergo a replacement reaction.

[0039] Please refer to Figure 2, a flow-type preparation device 100 of nanomaterials provided by the present invention includes a reactant container 1, a particle collector 2 arranged relative to the reactant container 1, a reaction channel 3 connected to both the reactant container 1 and the particle collector 2, a solution collector 4 connected to the particle collector 2, and a reflux mechanism 5 connected to both the solution collector 4 and the reactant container 1.

[0040] In the above structure, the reactant container 1 can contain a liquid or a solid-liquid mixture. The reactant container 1 is connected to the reaction channel 3. The solutions stored in the reactant container 1 flow into the reaction channel 3 simultaneously or sequentially according to a set sequence. The end of the reaction channel 3 is connected to the particle collector 2.

[0041] Specifically, the reactant container 1 includes a first reaction container 11, a first replenishing channel 12 and a first reflux port 13 arranged on two opposite sides of the first reaction container 11, a second reaction container 14 spaced apart from the first reaction container 11, a second replenishing channel 15 and a second reflux port 16 arranged on two opposite sides of the second reaction container 14, and a connecting pipe 17 connected to the bottom of both the first reaction container 11 and the second reaction container 14.

[0042] In this embodiment, two reaction vessels are provided: a first reaction vessel 11 and a second reaction vessel 14, but this is not limiting. The specific number of reaction vessels can be adjusted according to actual conditions, and the reaction vessels can contain liquids or solid-liquid mixtures. Furthermore, the reaction solution temperature can be controlled and stirred within the reaction vessels to ensure uniformity. Furthermore, a first replenishment channel 12 and a second replenishment channel 15 are provided around the first reaction vessel 11 and the second reaction vessel 1, respectively, to ensure timely and rapid replenishment of reactants, preventing reactant shortages.

[0043] Furthermore, the reaction channel 3 includes a water bath ultrasonic container 31 located between the connecting pipe 17 and the particle collector 4 and a hollow pipe 32 located in the water bath ultrasonic container 31, one end of the hollow pipe 32 is connected to the connecting pipe 17, and the other end of the hollow pipe 32 is connected to the particle collector 4.

[0044] In this embodiment, the hollow conduit 32 is linear or spiral in shape, and a flow rate control valve may be added to the hollow conduit 32 to more conveniently control the flow rate of the reaction solution in the hollow conduit 32. Furthermore, the water bath ultrasonic container 31 contains an aqueous solution, and the hollow conduit 32 is partially immersed in the aqueous solution contained in the water bath ultrasonic container 31. The water bath ultrasonic container 31 can apply ultrasound or temperature control to the hollow conduit 32 to promote full contact between the metal ion solution and the micro-nano metal solution to cause a replacement reaction.

[0045] Furthermore, the particle collector 2 includes a processing mechanism 21 connected to one end of the hollow pipe 32 away from the connecting pipe 17 and a particle collecting mechanism 22 that is detachably connected to the processing mechanism 21, the solution collector 4 is connected to the particle collecting mechanism 22, and the reflux mechanism 5 is simultaneously connected to the solution collector 4, the first reflux port 13 and the second reflux port 16.

[0046] In this embodiment, the number of the particle collection mechanisms 22 can be one or more, and is not limited thereto. Furthermore, if the processing mechanism 21 is a filter and / or a centrifuge, the nanomaterial particles are deposited in the particle collection mechanism 22 for collection. If the processing mechanism 21 is a centrifuge, the nanomaterial particles are deposited on the inner wall of the particle collection mechanism 22 for collection.

[0047] It is worth mentioning that the particle collection mechanism 22 and the processing mechanism 21 form a detachable connection, which facilitates the replacement of different collection modes to meet different collection needs. At the same time, the collected particles can also be removed by disassembly, which reduces time costs and improves production efficiency.

[0048] It should be noted that, referring to FIG3 , in another embodiment, the flow-type preparation device 100 of nanomaterials provided by the present invention can also disassemble the solution collector 4 and the reflux mechanism 5 , and can still achieve the large-scale flow-type continuous production of the above-mentioned nanomaterial particles.

[0049] Compared with the related art, the present invention provides a flow-type preparation method and device for nanomaterials. Under the setting of the communicating vessel principle, the metal ion solution and the micro-nano-scale metal solution undergo a replacement reaction in the reaction channel to form a reaction mixture solution. The reaction mixture solution includes a completely reacted solution and an unreacted solution. The reaction mixture solution then flows into a particle collector. The completely reacted solution forms the required nanomaterial particles, which will be adsorbed in the particle collector. The unreacted solution flows into the solution collector, and a reflux mechanism extracts the unreacted solution in the solution collector and refluxes the micro-nano-scale metal solution and the metal ion solution in the unreacted solution into corresponding reactant containers. The nanomaterial particles in the particle collector are then collected. The flow-type preparation method and device for nanomaterials provided by the present invention achieve large-scale flow-type continuous production of nanomaterial particles. At the same time, the completely reacted particles can be directly collected, effectively improving production efficiency and output. The method is particularly suitable for the industrial field and has good industrialization prospects.

[0050] The foregoing description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Those skilled in the art will readily appreciate that various modifications and variations of the present invention are possible. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the present invention are intended to be encompassed within the scope of the claims.

Claims

1. A continuous preparation method of nanomaterials, characterized in that: The preparation method comprises: Step S1, placing one or more metal ion solutions and micro-nano metal solutions in a reactant container; Step S2, respectively controlling the metal ion solution and the micro-nano metal solution to flow into the reaction channel at a specific flow rate at the same time, so that the metal ion solution and the micro-nano metal solution are fully in contact and undergo a replacement reaction to form a reaction mixed solution, wherein the reaction mixed solution includes a completely reacted solution and an unreacted completely solution; Step S3, controlling the completely reacted solution and the unreacted completely reacted solution to flow into a particle collector and a solution collector respectively; Step S4, drawing the unreacted complete solution from the solution collector through a reflux pipe and returning it to the reactant container; Step S5, looping the process from step S1 to step S4.

2. The continuous preparation method of nanomaterials according to claim 1, characterized in that: The micro-nano metal solution comprises micro-nano metal particles and a solvent.

3. The continuous preparation method of nanomaterials according to claim 2, characterized in that: The micro-nano metal particles are bidirectional metal particles.

4. The continuous preparation method of nanomaterials according to claim 2, characterized in that: The solvent includes deionized water and an organic solvent, and the organic solvent is an alcohol organic solvent or a ketone organic solvent.

5. The continuous preparation method of nanomaterials according to claim 1, characterized in that: The flow rate of the metal ion solution and the micro-nano metal solution flowing into the reaction channel is 4:1 or 1:1 or 2:

1.

6. The continuous preparation method of nanomaterials according to claim 1, characterized in that: In step 2, the reaction channel is controlled by applying any one of ultrasound, ultraviolet rays and high temperature to the metal ion solution and the micro-nano metal solution, so that the metal ion solution and the micro-nano metal solution are fully contacted and undergo a substitution reaction to form a reaction mixed solution.

7. A continuous preparation device for nanomaterials, characterized in that: The device includes a reactant container, a particle collector arranged relatively spaced apart from the reactant container, a reaction channel connected to both the reactant container and the particle collector, a solution collector connected to the particle collector, and a reflux mechanism connected to both the solution collector and the reactant container.

8. The continuous preparation device of nanomaterials according to claim 7, characterized in that: The reactant container includes a first reaction container, a first replenishing channel and a first reflux port arranged on two opposite sides of the first reaction container, a second reaction container spaced apart from the first reaction container, a second replenishing channel and a second reflux port arranged on two opposite sides of the second reaction container, and a connecting pipe connected to the bottom of both the first reaction container and the second reaction container.

9. The continuous preparation device of nanomaterials according to claim 8, characterized in that: The reaction channel includes a water bath ultrasonic container located between the connecting pipe and the particle collector and a hollow pipe located in the water bath ultrasonic container, one end of the hollow pipe is connected to the connecting pipe, and the other end of the hollow pipe is connected to the particle collector; the shape of the hollow pipe is linear or spiral.

10. The continuous preparation device of nanomaterials according to claim 9, characterized in that: The particle collector includes a processing mechanism connected to one end of the hollow pipe away from the connecting pipe and a particle collecting mechanism that is detachably connected to the processing mechanism. The solution collector is connected to the particle collecting mechanism, and the reflux mechanism is simultaneously connected to the solution collector, the first reflux port and the second reflux port; the processing mechanism is a suction filter and / or a centrifuge.

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